Extracurricular laboratory: Synthetic route of 15441-07-3

The synthetic route of Methyl 3-(chlorosulfonyl)propanoate has been constantly updated, and we look forward to future research findings.

Application of 15441-07-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 15441-07-3, name is Methyl 3-(chlorosulfonyl)propanoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[0586] Preparation of 53 [0587] To a solution of 52 (0.08 g, 0.395 mmol) in CH2Cl2 (3 mL), added pyridine (74 muL) and methyl 3-(chlorosulfonyl)propanoate (0.1 g, 0.544 mmol). Reaction mixture was stirred for 16 h at rt. and then poured in 10% HCl solution followed by extraction with CH2Cl2. Organic layer was dried and evaporated to obtained 53 (52mg, 34%).

The synthetic route of Methyl 3-(chlorosulfonyl)propanoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Cambridge Enterprise Limited; Kapadnis, Prashant Bhimrao; Glen, Robert; Hiley, Robin; Bell, James; Spring, David; US2013/53372; (2013); A1;,
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Share a compound : 79669-50-4

According to the analysis of related databases, 79669-50-4, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 79669-50-4 as follows. SDS of cas: 79669-50-4

Compound BB-4A-2 (1.00 g, 4.37 mmol), compound BB-1A (1.40 g, 4.37 mmol) and potassium carbonate (1.81 g, 13.10 mmol) were dissolved in 1,4-dioxane (10 mL) and water (3 mL) under nitrogen atmosphere, followed by addition of (1,1′-bis(diphenylphosphino)ferrocene)palladium dichloride dichloromethane complex (356.50 mg, 436.55 mumol). The reaction mixture was stirred for 10 hours at 90 C under nitrogen atmosphere. After completion of the reaction, the reaction solution was cooled to room temperature and concentrated under reduced pressure, followed by addition of water (10 mL) and extraction with ethyl acetate (10 mL¡Á3). The organic phases were combined, washed with saturated brine (30 mL), dried over anhydrous sodium sulfate, filtered to remove the desiccant and concentrated under reduced pressure. The insoluble material was removed by filtration, and the obtained residue was purified by column chromatography (eluent: petroleum ether/ethyl acetate=100/1, 9/1) to obtain the title compound BB-4A-3 (yellow solid, 1.00 g, yield 59.74%). 1H NMR (400MHz,CDCl3) delta: 8.03 (d, J=2.0 Hz, 1H), 7.51 (dd, J=1.9, 7.9 Hz, 1H), 7.45 (d, J=8.8 Hz, 2H), 7.21 – 7.17 (m, 1H), 6.93 (d, J=8.8 Hz, 2H), 4.11 – 4.08 (m, 2H), 3.84 (s, 3H), 3.74 (t, J=4.9 Hz, 2H), 3.48 (t, J=6.7 Hz, 2H), 2.55 (s, 3H), 1.55 – 1.50 (m, 2H), 1.36 – 1.28 (m, 2H), 0.86 (t, J=7.4 Hz, 3H).

According to the analysis of related databases, 79669-50-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Medshine Discovery Inc.; LUO, Yunfu; BA, Yuyong; CHEN, Shuhui; (135 pag.)EP3567028; (2019); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

A new synthetic route of 6091-64-1

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 2-bromobenzoate, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 6091-64-1, name is Ethyl 2-bromobenzoate, belongs to esters-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 6091-64-1, Quality Control of Ethyl 2-bromobenzoate

General procedure: Then, the corresponding ester was refluxed with 85% hydrazine monohydrate in ethanol to get hydrazide 1.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 2-bromobenzoate, and friends who are interested can also refer to it.

Reference:
Article; Li, Chao; Liu, Jia-Chun; Li, Ya-Ru; Gou, Cheng; Zhang, Mei-Ling; Liu, Hong-Yan; Li, Xiao-Zhen; Zheng, Chang-Ji; Piao, Hu-Ri; Bioorganic and Medicinal Chemistry Letters; vol. 25; 15; (2015); p. 3052 – 3056;,
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Ester – an overview | ScienceDirect Topics

Discovery of 52727-57-8

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-amino-5-bromobenzoate, its application will become more common.

Related Products of 52727-57-8,Some common heterocyclic compound, 52727-57-8, name is Methyl 2-amino-5-bromobenzoate, molecular formula is C8H8BrNO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

(iii) Methyl 5-bromo-2-({[3-(furan-3-yl)phenoxy]acetyl}amino)benzoate Under ice-cooling, 1.53 g (7.97 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added to a DMAc (5 mL) solution comprising 1.45 g (6.64 mmol) of [3-(furan-3-yl)phenoxy]acetic acid, 1.60 g (6.97 mmol) of methyl 2-amino-5-bromobenzoate, and 1.08 g (7.97 mmol) of 1-hydroxybenzotriazole, and the mixture was stirred at room temperature for 4 hours. Under ice-cooling, 1.63 g (19.9 mmol) of 1-methylimidazole was added, and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, and the mixture was stirred for 1 hour. The precipitates were collected by filtration and washed with water and IPE, followed by drying under reduced pressure at 50 C. for 3 hours, thereby giving 2.30 g of methyl 5-bromo-2-({[3-(furan-3-yl)phenoxy]acetyl}amino)benzoate (yield: 81%). 1H-NMR (CDCl3) delta: 3.97 (3H, s), 4.68 (2H, s), 6.72 (1H, dd, J=1.7, 1.0 Hz), 6.97 (1H, ddd, J=7.9, 2.6, 1.0 Hz), 7.19 (1H, ddd, J=7.9, 1.5, 1.0 Hz), 7.23 (1H, dd, J=2.6, 1.5 Hz), 7.35 (1H, t, J=7.9 Hz), 7.49 (1H, t, J=1.7 Hz), 7.67 (1H, dd, J=9.0, 2.4 Hz), 7.76 (1H, dd, J=1.4, 1.0 Hz), 8.19 (1H, d, J=2.4 Hz), 8.74 (1H, d, J=9.0 Hz), 12.08 (1H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-amino-5-bromobenzoate, its application will become more common.

Reference:
Patent; RENASCIENCE CO., LTD.; US2012/22080; (2012); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

The important role of 99548-54-6

The chemical industry reduces the impact on the environment during synthesis Methyl 3-bromo-2-methylbenzoate. I believe this compound will play a more active role in future production and life.

Reference of 99548-54-6, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 99548-54-6, name is Methyl 3-bromo-2-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of methyl 3-bromo-2-methylbenzoate (500 mg, 3.3 mmol), NBS (770.4 mg, 4.3 mmol), and di-benzoyl peroxide (BPO, 80.7 mg, 0.3 mmol) in 1,2-dichloroethane (10 mL) was heated at 80 C for 12 h. The reaction mixture was cooled to room temperature, and the precipitated solid was removed by filtration and washed with ethers (10 mL). The filtrate was concentrated in vacuo and the residue was partitioned between 2 N NaHCO3 (15 mL) and ethers (15 mL). The organic layer was separated, dried over NaSO4, filtered and concentrated to give a crude product (683.2 mg, 89.6%), which was used in the next step reaction without further purification.

The chemical industry reduces the impact on the environment during synthesis Methyl 3-bromo-2-methylbenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Article; Li, Qing; Meng, Liuwei; Zhou, Siru; Deng, Xiaoyan; Wang, Na; Ji, Yi; Peng, Yichun; Xing, Junhao; Yao, Gongmei; European Journal of Medicinal Chemistry; vol. 180; (2019); p. 509 – 523;,
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New downstream synthetic route of 105-53-3

According to the analysis of related databases, 105-53-3, the application of this compound in the production field has become more and more popular.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 105-53-3, name is Diethyl malonate, This compound has unique chemical properties. The synthetic route is as follows., Safety of Diethyl malonate

[Reference Example 3] Production of 1,1-di-ethoxycarbonyl-2-vinylcyclopropane 8.79 g (54.9 mmol) of diethyl malonate and 99 mL of toluene were added into a three-necked flask (300 mL), and thereafter, 20.5 mL (52.4 mmol) of a 20% sodium ethoxide ethanol solution was added thereto as a base. The obtained mixture was stirred at room temperature for 0.5 hours. Thereafter, 9.89 g (24.9 mmol) of cis-1,4-di-4-toluenesulfonyloxy-2-butene, which had been obtained by performing the same operations as those in Example 1 and then purifying the obtained compound by silica gel chromatography, was added to the reaction solution. The obtained mixture was stirred at room temperature for 3.5 hours, and thereafter, 59.9 mL of a 1 M sodium hydroxide aqueous solution was added to the reaction solution. The obtained mixture was stirred for 1 hour, and an organic layer was then separated. A water layer was re-extracted with 50 mL of toluene, and organic layers were gathered. The gathered organic layer was washed with 50 mL of water three times, and the resultant was then filtrated, while washing the residue with toluene. The obtained filtrate was concentrated at 45C under reduced pressure, so as to obtain 22.4 g of 1,1-di-ethoxycarbonyl-2-vinylcyclopropane in the form of a crude product of a light yellow oily substance. This crude product contained 1.25 g of 1,1-di-ethoxycarbonyl-2-vinylcyclopropane (yield: 24%) and 3.94 g of 1,1-di-ethoxycarbonyl-3-vinylcyclopentene (yield: 74%).

According to the analysis of related databases, 105-53-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; API Corporation; EP2537825; (2012); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Share a compound : 107045-28-3

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 107045-28-3, name is tert-Butyl 4-(aminomethyl)benzoate, A new synthetic method of this compound is introduced below., Quality Control of tert-Butyl 4-(aminomethyl)benzoate

To a stirred solution of 5-chloro-2-hydroxybenzoic acid (0.57 g, 3.3 mmol) and tert-butyl 4-(aminomethyl)benzoate (0.72 g, 3.5 mmol) in dichloromethane (5 mL) were successively added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCl) (0.95 g, 5.0 mmol), 1-hydroxybenzotriazole hydrate (HOBT) (0.76 g, 5.0 mmol), and triethylamine (0.46 mL, 3.3 mmol). After being stirred overnight, the reaction mixture was poured into sodium bicarbonate aqueous solution (50 mL). The organic layer was separated, and the aqueous layer was extracted with dichloromethane (20 mL*2). The combined organic layers were washed with brine (50 mL), dried (magnesium sulfate), and evaporated. The residue was purified by flush column chromatography on silica gel eluding with hexane/ethyl acetate (10/1) to afford 0.57 g (48%) of the title compound as white solids: 1H-NMR (CDCl3) delta 12.12 (1H, s), 7.99 (2H, d, J=7.9 Hz), 7.47-7.30 (4H, m), 6.97 (1H, d, J=8.4 Hz), 6.67-6.52 (1H, m), 4.68 (2H, d, J=5.7 Hz), 1.59 (9H, s).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Pfizer Inc; US2005/250818; (2005); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Some tips on 39503-58-7

The chemical industry reduces the impact on the environment during synthesis Methyl 5-bromo-2-methoxy-4-methylbenzoate. I believe this compound will play a more active role in future production and life.

Reference of 39503-58-7, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 39503-58-7, name is Methyl 5-bromo-2-methoxy-4-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows.

The bromo derivative from above (44.5 g, 0.17 mol) was added in small portions to conc. H2SO4 (170 mL) and the mixture was stirred in an ice-salt bath until all SOLIDS DISSOLVED. CONC. HN03 (17 mL) was then added dropwise over 20 min and stirring continued for an additional hour in the ice bath. The reaction mixture was then slowly added to ice-water (2 L) and the precipitated yellow solid was collected by filtration. The solid was washed with water, NAHC03 solution and water again. After drying, the desired nitro derivative was obtained as an orange solid (36.8 g).

The chemical industry reduces the impact on the environment during synthesis Methyl 5-bromo-2-methoxy-4-methylbenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO KG; WO2004/65367; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Analyzing the synthesis route of 106-32-1

The synthetic route of 106-32-1 has been constantly updated, and we look forward to future research findings.

Reference of 106-32-1,Some common heterocyclic compound, 106-32-1, name is Ethyl octanoate, molecular formula is C10H20O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Ethyl octanoate (105 g, 0.61 mol) was dissolved in methanol (420 mL, 4 V) and stirred, then pumped into the coil with pump A at a rate of 5.6 g/min, sodium borohydride (33.86 g, 0.92 mol), EtONa (1.24g, 0.018mol) was dissolved in methanol (105mL, 1V) and pumped to a 240mL coil with pump B at a rate of 1.5g / min. The coil was immersed in a 40 C oil bath, and the outlet was sampled by HPLC. The system was subjected to quenching extraction in a 2 L four-necked flask and subjected to column chromatography to obtain 70 g of a product in a yield of 80%.

The synthetic route of 106-32-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kailaiying Pharmaceutical Group (Tianjin) Co., Ltd.; Hong Hao; Lu Jiangping; Zhang Enxuan; Liu Zhiqing; Zhang Tao; (21 pag.)CN110156549; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

The important role of 15568-85-1

The synthetic route of 15568-85-1 has been constantly updated, and we look forward to future research findings.

Related Products of 15568-85-1, These common heterocyclic compound, 15568-85-1, name is 5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

4-Methoxyaniline (1.27 g) and 5-methoxymethylene-2,2-dimethyl-[1,3]dioxan-4,6-dione (1.82 g) were dissolved in 2-propanol (40 ml), and the solution was stirred at 50C for 2 hr. The solvent was removed by distillation under the reduced pressure, and the residue was washed with ether to give 5-[(4-methoxy-phenylamino)-methylene]-2,2-dimethyl-[1,3]dio xan-4,6-dione (1.98 g, yield 73%). 5-[(4-Methoxy-phenylamino)-methylene]-2,2-dimet hyl-[1,3]dioxan-4,6-dione (1.28 g) and biphenyl (5.2 g) were suspended in diphenyl ether (20 ml), and the suspension was stirred at 220C for one hr. The reaction mixture as such was purified by column chromatography with a methanol-chloroform system to give 6-methoxy-1H-quinolin-4-one (398 mg, yield 49%). 6-Methoxy-1H-quinolin-4-one (398 mg) was suspended in diisopropylethylamine (3 ml), phosphorus oxychloride (1 ml) was added to the suspension, and the mixture was stirred at 100C for one hr. Water was added to the reaction mixture under ice cooling, and the aqueous layer was neutralized with an aqueous sodium hydrogencarbonate solution. The organic layer was extracted with ethyl acetate, and the ethyl acetate layer was washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography with an acetone-chloroform system to give 4-chloro-6-methoxyquinoline (375 mg, yield 42%).

The synthetic route of 15568-85-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KIRIN BEER KABUSHIKI KAISHA; EP1724268; (2006); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics