Tag: M.W=200-300

Adding a certain compound to certain chemical reactions, such as: 957207-58-8, name is Methyl 4-bromo-2-(trifluoromethyl)benzoate, 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 957207-58-8, COA of Formula: C9H6BrF3O2

To a solution of methyl 4-bromo-2-(trifluoromethyl)benzoate (537 mg, 1.67 mmol) in 13 mL of toluene was added at room temperature cyclopropylboronic acid (220 mg, 2.56 mmol), K3PO4 (641 mg, 3.02 mmol), water (0.4 mL) and Pd(Ph3)4 (193 mg, 0.167 mmol) and the resulting mixture was degassed for 10 minutes with a stream of N2. The reaction mixture was stirred at 110 C for 7 hours. Water was added and product was extracted with ethyl acetate (three times). The collected organic layers were dried over Na2SO4, filtered and evaporated in high vacuum to yield methyl 4-cyclopropyl-2-(trifluoromethyl)benzoate (crude, 802 mg) as agrey solid. MS found for C12H11F3O2 as (M+H)+ 245.0.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 4-bromo-2-(trifluoromethyl)benzoate, and friends who are interested can also refer to it.

Reference:
Patent; PHARMACYCLICS LLC.; ATALLAH, Gordana, Babic; CHEN, Wei; JIA, Zhaozhong, J.; POZZAN, Alfonso; RAVEGLIA, Lucal, Francesco; ZANALETTI, Riccardo; (815 pag.)WO2016/196776; (2016); A2;,
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Reference of 26759-46-6, 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. 26759-46-6, name is Methyl 2-amino-4,5-dimethoxybenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 11 Benzoic acid, 2,2′-dithiobis[4,5-dimethoxy-, dimethyl ester To a suspension of methyl 2-amino-4,5-dimethoxy-benzoate (1.50 g, 7.11 mmol) in acetic acid (10 mL) and conc. HCl (13 mL) at an internal temperature of 1¡ã-3¡ã C. was slowly added a solution of sodium nitrite (0.55 g, 7.97 mmol) in water (5 mL); the solid went into solution upon the final addition of the aqueous sodium nitrite. The solution was stirred for an additional 30 minutes. and then sulphur dioxide was bubbled through the cold solution for 30 minutes. Cupric chloride dihydrate (0.471 g, 2.76 mmol) in water (5 mL) was added and the green mixture allowed to warm to room temperature over 48 hours. Filtration and washing with water (3*100 mL) afforded the required product as a white solid (0.800 g, 49percent). Analysis calc’d for C20 H22 O8 S2: C, 52.85; H, 4.88; Found: C, 52.64; H, 4.89. MS (CI) m/e 454.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 2-amino-4,5-dimethoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Warner-Lambert Company; US5599811; (1997); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 7686-78-4,Some common heterocyclic compound, 7686-78-4, name is Diethyl 2-vinylcyclopropane-1,1-dicarboxylate, molecular formula is C11H16O4, 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.

Preparation method: In air atmosphere,Add 0.2 mmol of N-pyrimidindolline compound to the microwave reaction tube,0.36 mmol of ethylene cyclopropane compound,0.008mmol of [Ru (p-cymene) Cl2] 2,0.08 mmol mesitylene,0.04mmol of silver hexafluoroantimonate, microwave reaction at 60 C for 1 hour;After completion of the reaction, rinse with ethyl acetate.Chromatographic separation after concentration under reduced pressure (silica gel 200-300 mesh, eluent: ethyl acetate / petroleum ether gradient elution, ratio from 0/100 to 100/0)Dried to a pale yellow oil,Yield: 81%, E / Z> 20: 1.

The synthetic route of 7686-78-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhengzhou University; Henan Communication Polytechnic College; Zhu Xinju; Wang Qiuling; Xie Xiaona; Zhang Xiaojie; Yan Jing; Xu Yan; Hao Xinqi; Song Maoping; (15 pag.)CN110551106; (2019); A;,
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Related Products of 82702-31-6, These common heterocyclic compound, 82702-31-6, name is Methyl 3-bromo-4-fluorobenzoate, 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.

To a solution of Example 35a (1.86 g, 13.27 mmol) and methyl 3-bromo-4- fluorobenzoate (2.099 mL, 14.20 mmol) in dimethyl sulfoxide (14 mL) was added cesium carbonate (6.49 g, 19.91 mmol). The mixture was heated at 80 C for 2 hours, cooled, and diluted with water (100 mL), then extracted with methyl tert-butyl ether (200 mL). The aqueous phase was extracted with additional portions (2 x 100 mL) of methyl tert-butyl ether.The combined organics were dried over anhydrous sodium sulfate, filtered, and concentrated. The crude material was purified by chromatography (silica gel, eluting with 0-25 % ethyl acetate/heptanes) to provide 4.56g (97%) of the title compound.

The synthetic route of 82702-31-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBVIE INC.; ABBVIE PHARMACEUTICAL TRADING (SHANGHAI) CO., LTD.; FIDANZE, Steven D.; HASVOLD, Lisa A.; LIU, Dachun; MCDANIEL, Keith F.; PRATT, John; SCHRIMPF, Michael; SHEPPARD, George S.; WANG, Le; LI, Bing; (191 pag.)WO2017/177955; (2017); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 6942-37-6, name is Methyl 5-amino-2-bromobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: Methyl 5-amino-2-bromobenzoate

Step B. Preparation of methyl 2-bromo-5-(dimethylamino)benzoateTo a stirred solution of 5-amino-2-bromo-benzoic acid methyl ester (3.30 g, 14.35 mmol) in CH3OH (45 mL) containing CH2O (3.6 mL, 45.0 mmol) at room temperature was added a solution of NaBH3CN (945 mg, 14.35 mmol) and ZnCI2 (990 mg, 7.2 mmol) in CH3OH (45 mL). The reaction mixture was stirred at room temperature overnight, then concentrated. The residue was taken up in 0.1 N NaOH solution, extracted with EtOAc several times. The combined extracts were washed with H2O, brine, dried over dried Na2SO4, then filtered and concentrated. The residue was separated by silica gel column (hexane/EtOAc = 3 : 1) to give 2.991 g (92%) of methyl 2-bromo-5-(dimethylamino)benzoate as a yellow oil based on the partial recovery of (412 mg). methyl 2-bromo-5-(dimethylamino)benzoate, MS: m/z 259 (M + H)

The synthetic route of 6942-37-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; WYETH; WO2009/120826; (2009); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 105-76-0, name is Dibutyl maleate, A new synthetic method of this compound is introduced below., Safety of Dibutyl maleate

EXAMPLE 31 Synthesis of Dibutyl 5-EPDC from Hydroxylamine, Dibutyl Maleate, and 2-Ethylacrolein Hydroxylamine free base (50% aqueous solution, 8.0 g, 0.12 mol) was added dropwise to dibutyl maleate (25.0 g, 0.1 mol) in a 3-necked 250-ml flask blanketed with nitrogen. The reaction temperature was maintained below 55 C. with an ice bath. The mixture was stirred for 30 minutes and then analyzed by NMR, which indicated 96% conversion of dibutyl maleate to dibutyl N-hydroxyaspartate. Butanol (29.8 g), hexadecane (0.98 g), 2-ethylacrolein (10.0 g, 0.12 mol), and trifluoroacetic acid (2.0 g, 0.018 mol) were added in succession to the reaction mixture, which was then stirred at 90-95 C. for 4.5 hours under nitrogen.

The synthetic route of 105-76-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoechst Celanese Corporation; US5322948; (1994); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 15448-76-7, These common heterocyclic compound, 15448-76-7, name is Dimethyl bicyclo[2.2.1]heptane-1,4-dicarboxylate, 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.

[1268A solution of sodium hydroxide (940 mg) in methanol (10 mL) was added to a solution of dimemylbicyclo[2.2.1]heptane-l,4-dicarboxylate (5.00 g) in THF (150 mL), and the resultant was stirred overnight at room temperature. The reaction mixture was distilled off under reduced pressure, the obtained residue was dissolved in water, and extraction thereof was performed using dichloromethane. A pH of the obtained aqueous layer was set to pH 3 using 6 M hydrochloric acid, and extraction thereof was performed using ethyl acetate. The obtained organic layer was distilled off under reduced pressure, thereby obtaining the title compound (2.50 g). 1H MR (400 MHz, DMSO-d^ 1.57-1.63 (4H, m), 1.72 (2H, s), 1.91-1.92 (4H, m), 3.60 (3H, s), 12.21 (lH, s).

The synthetic route of 15448-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; KASAI, Shizuo; OGINO, Masaki; MIZOJIRI, Ryo; YAMASAKI, Takeshi; HIROSE, Hideki; TAKAKURA, Nobuyuki; YAMASHITA, Tohru; MORIMOTO, Sachie; NAKAHATA, Takashi; KINA, Asato; WO2014/142363; (2014); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

4131-74-2, name is Dimethyl 3,3-Thiodipropionate, belongs to esters-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: Dimethyl 3,3-Thiodipropionate

2.7098 g of NaH (60%) was added to 250 ml of dry three-necked flask,40 ml of anhydrous tetrahydrofuran (THF) was added,Stirred at room temperature for 10 min,A solution of dimethyl 3,3′-thiodipropionate (10.1015 g)In THF (30 ml) was added and heated to reflux,About 1h drops finished,After adding 10mlTHF rinse the dropping funnel,Continue to return after 1h,The reaction was stopped and allowed to cool to room temperature.The reaction solution was adjusted to a pH of 6 to 7 with 2% dilute hydrochloric acid and then extracted with dichloromethane (30 ml * 3)The layers were washed with saturated sodium chloride solution and the organic layer was collected and washed with sufficient anhydrous sodium sulfate and filtered. The filtrate was filteredThe solvent was removed by evaporation to give 7.5639 g of a yellow oily liquid,4-oxo-tetrahydro-2H-thiopyran-3-carboxylic acid methyl ester (II)Yield 88.7%.

The synthetic route of 4131-74-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangxi Science and Technology Normal University; Zhu Wufu; Zheng Pengwu; Sun Chengyu; Tang Qidong; Chen Chen; Lei Fei; Wu Chunjiang; Tu Yuanbiao; Ouyang Yiqiang; (42 pag.)CN105153190; (2017); B;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 23877-12-5, name is tert-Butyl 2-bromo-2-methylpropanoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: esters-buliding-blocks

59.1) tert-butyl 2-methyl-2-(10H-phenothiazin-2-yloxy)propanoate: 1.93 g (3 eq.) of K2CO3 is added to a solution of 1 g (4.6 mmol) of intermediate 21.1 in 10 ml of DMF. The reaction mixture was heated to 60 C. before the addition of 1.73 ml (2 eq.) of tert-butyl 2-bromoisobutyrate. The mixture is then taken to 110 C. and stirring is maintained at this temperature for 6 hours. After returning to 20 C., the mixture is poured into 100 ml of water and the product is extracted using twice 100 ml of ethyl acetate. The organic solution is finally washed with 100 ml of salt water, dried over sodium sulphate, filtered and concentrated to dryness under vacuum. The evaporation residue is purified on a silica column, eluent: ethyl acetate/heptane (1/9). 450 mg of a pale pink solid is obtained with a yield of 28%. Melting point: 138-140 C.

The synthetic route of 23877-12-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Auvin, Serge; Chabrier De Lassauniere, Pierre-Etienne; US2005/222045; (2005); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 681465-85-0, The chemical industry reduces the impact on the environment during synthesis 681465-85-0, name is Methyl 4-amino-3-isopropoxybenzoate, I believe this compound will play a more active role in future production and life.

To 10-Chloro-2-cyclopentyl-6-methyl-2,6,9,11-tetrazabicyclo[5.4.0]undeca-8,10,12-trien-5-one (Intermediate 1, 190 mg, 0.68 mmol) was added a solution of Methyl4-amino-3-propan-2-yloxy-benzoate (Intermediate 71, 145 mg, 0.69 mmol) in ethanol (4 mL), followed by water (12 mL). Concentrated hydrochloric acid (36%; 140 mul) was added and the reaction heated to 80 C., with stirring, overnight. The reaction was allowed to stand and cool overnight, before evaporating ethanol. The aqueous residue was diluted to 40 mL with water and the solution basified to pH 9 by addition of a few drops of aq. ammonia, The resultant emulsion was treated with a little brine and extracted with DCM (2¡Á30 mL). The biphasic mixture was poured into a PTFE cup and the organic phase allowed to drip through under gravity. Evaporation of the organic phase afforded an amber gum, which was purified by flash chromatography on silica (40 g Si cartridge; ISCO companion), eluting with a rising gradient of 25-100% ethyl acetate in iso-hexane. Product containing fractions were combined and evaporated to give a colourless gum which was triturated with a small amount of diethyl ether and the resultant solid collected by suction filtration and dried to afford the title compound as a white solid (132 mg, 43%)1H NMR (400.132 MHz, DMSO-D6) delta 1.36 (d, 6H), 1.58-1.77 (m, 6H), 1.95 (m, 2H), 2.60 (m, 2H), 3.18 (s, 3H), 3.64 (m, 2H), 3.83 (s, 3H), 4.77 (m, 2H), 7.53 (m, 1H), 7.57 (m, 1H), 7.78 (s, 1H), 8.10 (s, 1H), 8.51 (d, 1H); MS m/z 452 [M+H]+.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 4-amino-3-isopropoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; US2008/9482; (2008); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics