Tag: M.W=200-300

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. 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, A new synthetic method of this compound is introduced below., Product Details of 609-12-1

Example 53N-Hydroxy-2-(4-methoxy-benzenesulfonyl)-3-methyl-butyramide 2-(4-Methoxy-phenylsulfanyl)-3-methyl-butyric acid ethyl ester was prepared according to the general method as outlined in Example 1. Starting from ethyl 2-bromo-3-methyl-butanoate (20.9 g, 100 mmol) and 4-methoxybenzenethiol (14.0 g, 100 mmol), 30 g of 2-(4-methoxy-phenylsulfanyl)-3-methyl-butyric acid ethyl ester was isolated. Yield 99%; Light yellow oil; MS: 269 (M+H)+.

The synthetic route of 609-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wyeth Holdings Corporation; EP970046; (2003); B1;,
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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. 252881-74-6, name is tert-Butyl 3-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)propanoate, A new synthetic method of this compound is introduced below., Formula: C13H27NO5

A solution of 2-(2,6-dioxopiperidin-3-yl)-4- fluoroisoindoline- 1 ,3-dione (100 mg, 0.362 mmol), tert-butyl 3-(2-(2-(2-aminoethoxy)ethoxy) ethoxy)propanoate (100 mg, 0.362 mmol) and DIPEA (0.5 ml) in DMF (5 ml) was heated at 100 C overnight. After the starting materials were consumed, the reaction was concentratedunder reduced pressure. The resulting residue was purified by prep-HPLC to yield the product(72 mg, 37%) as yellow solid. ?H NMR (600 MHz, CD3OD) oe 7.55 (dd, J 7.1, 8.6 Hz, 1H),7.10 (d, J 8.5 Hz, 1H), 7.05 (d, J 7.0 Hz, 1H), 5.06 (dd, J= 5.4, 12.4 Hz, 1H), 4.10 (q, J=7.1 Hz, 1H), 3.72 (t, J 5.3 Hz, 2H), 3.69-3.59 (m, 8H), 3.59-3.55 (m, 2H), 3.50 (t, J= 5.3Hz, 2H), 2.91 -2.82 (m, 1H), 2.78-2.68 (m, 2H), 2.45 (t, J= 6.2 Hz, 2H), 1.43 (s, 9H). HRMS(ESI-TOF) m/z: [M+Hj calculated for C26H36N309, 534.2446; found: 534.2459.

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; ICAHN SCHOOL OF MEDICINE AT MOUNT SINAI; JIN, Jian; YANG, Xiaobao; LIU, Jing; XIONG, Yan; POULIKAKOS, Poulikos; KAROULIA, Zoi; WU, Xuewei; AHMED, Tamer; (199 pag.)WO2018/106870; (2018); A1;,
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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. 91085-56-2, name is Ethyl 3,5-dichlorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of Ethyl 3,5-dichlorobenzoate

Ethyl 3,5-dichlorobenzoate (8.4 g, 38.3 mmol) and sodiumhydride (1.1 g, 46.0 mmol) were dissolved in 100 mL THF underN2. To the mixture was added 13.2 mL ethyl propionate slowly atroom temperature and refluxed overnight. The solvent wasremoved under reduced pressure. The residue was extracted withethyl acetate, washed with water and brine and dried over Na2SO4.Flash column chromatography gave 9.7 g (92%) ethyl 3-(3,5-dichlorophenyl)-2-methyl-3-oxopropanoate 5 as orange solid. 1HNMR (400 MHz, DMSO-d6) d 7.97 (t, J = 3.3 Hz, 3H), 4.80 (q, J =6.9 Hz, 1H), 4.07 (q, J = 7.1 Hz, 2H), 1.31 (d, J = 6.9 Hz, 3H), 1.08(t, J = 7.1 Hz, 3H). MS (ESI, m/z): 274.0 [MH].

The synthetic route of 91085-56-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shu, Shuangjie; Dai, Antao; Wang, Jiang; Wang, Bin; Feng, Yang; Li, Jia; Cai, Xiaoqing; Yang, Dehua; Ma, Dakota; Wang, Ming-Wei; Liu, Hong; Bioorganic and Medicinal Chemistry; vol. 26; 8; (2018); p. 1896 – 1908;,
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Reference of 55666-43-8, The chemical industry reduces the impact on the environment during synthesis 55666-43-8, name is tert-Butyl 3-bromopropanoate, I believe this compound will play a more active role in future production and life.

5. To a solution of alcohol 3 (12.8 g, 40.84 mmol) in toluene (200 ml) was added Bu4NCI (3.7 g, 13.48 mmol). The reaction mixture was cooled to 0 0C after which aqueous 35% NaOH (250 ml) was added followed by a dropwise addition of tert- butyl 3-bromopropionate (4, 8.2 ml, 49.01 mmol) in toluene (50 ml). The mixture was stirred overnight at room temperature. The organic layer was separated and washed with H?O until neutral, dried (Na2SO4), concentrated and co-evaporated with CH2CI2 (3x). Purification by column chromatography (silica, heptane/EtOAc 4:1) gave 5 (11.2 g, 62%) as a yellow oil.

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, tert-Butyl 3-bromopropanoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GRUeNENTHAL GMBH; WO2009/124746; (2009); A1;,
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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. 39149-80-9, name is tert-Butyl 2-bromopropanoate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: tert-Butyl 2-bromopropanoate

General procedure: A solution of NaHMDS (1.0 M in THF, 2.1 mL, 2.1 mmol) was added dropwise to the solution of 15 (R4 and R5 are methyl, 334 mg, 2.0 mmol) in THF (10 mL) at 78 C under argon. After 5 min, a solution of 16 (152 mg, 1.0 mmol) in THF (5 mL) was added dropwise. After another 5 min, the reaction was quenched with saturated ammonium chloride solution. The aqueous phase was extracted with EtOAc (3 20 mL). The combined organic layer was washed with saturated brine and dried over Na2SO4. The solvent was removed under reduced pressure

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 39149-80-9.

Reference:
Article; Li, Qing; Xiao, Fenfen; Wang, Yunxia; Hu, Xiangdong; Synthetic Communications; vol. 46; 12; (2016); p. 1062 – 1067;,
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Synthetic Route of 35450-36-3, 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. 35450-36-3, name is Methyl 2-bromo-5-methoxybenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A sealed tube of 25 mL equipped with a magnetic stir bar was charged with alkynes (0.20 mmol), 2-bromobenzoic esters (0.22 mmol), CuI (0.02 mmol, 10 mol%), NaOH (0.4 mmol, 2 equiv) and CH3CN (1.0 mL). The reaction mixture was stirred at 100 C for 24 h. The reaction was monitored by GC or GC-MS. After completion of the reaction, the reaction mixture was cooled to room temperature, then washed with saturated NH4Cl aqueous solution (5.0 mL), and extracted with CHCl3 (3 * 5.0 mL). The combined organic phases were dried over Na2SO4 (anhydrous), concentrated in vacuum. The crude product was purified by flash column chromatography (eluent: ethyl acetate/petroleum ether = 1/20-1/10) on silica gel to afford the desired product.

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-bromo-5-methoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Sun, Mengli; Su, Lebin; Dong, Jianyu; Liu, Long; Zhou, Yongbo; Yin, Shuang-Feng; Tetrahedron Letters; vol. 58; 25; (2017); p. 2433 – 2437;,
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Reference of 169044-96-6, 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. 169044-96-6, name is Methyl 2-amino-5-bromo-4-methoxybenzoate, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of compound 35 (500 mg, 1.92 mmol) inDMF (10 mL) were added 4,4,5,5-tetramethyl-2-(3-methylbut-2-enyl)-1,3,2-dioxaborolane (452 mg,2.31 mmol), Pd(dppf)2Cl2 (140 mg, 0.19 mmol) andCs2CO3 (1253 mg, 3.85 mmol). The mixture was stirred at70 C for 24 h with the protection of N2. It was cooled to RTand diluted with water and extracted with ethyl acetate. Thecombined organic layers were washed with brine. It wasdried over Na2SO4 and filtered. The filtrate was concentratedand the residue was purified by silica gel columnchromatography eluting with cyclohexane/EA (uv254,20:1) to give pale-yellow powder 36 (198.0 mg, 43.0%). 36:1H NMR (500 MHz, CDCl3) delta 7.63 (s, 1H), 7.35 (dd, J =8.6, 4.2 Hz, 4H), 6.94 (dd, J = 24.0, 8.6Hz, 4H), 6.07 (s,1H), 5.26 (t, J = 7.3 Hz, 1H), 4.99 (s, 2H), 4.64 (dd, J =13.8, 3.5 Hz, 1H), 4.41 (s, 1H), 3.81 (s, 3H), 3.80 (s, 3H),3.19 (d, J = 7.3 Hz, 2H), 2.78 (dd, J = 16.1, 13.9 Hz, 1H),2.65 (dd, J = 16.2, 2.7 Hz, 1H), 1.72 (s, 3H), 1.69 (s, 3H).

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

Reference:
Article; Yi, Jingyu; Du, Guoxin; Zhao, Yuanyuan; Zhang, Liuqiang; Li, Bo; Zhu, Weiliang; Huang, Cheng; Li, Yiming; Guo, Fujiang; Medicinal Chemistry Research; vol. 27; 7; (2018); p. 1851 – 1862;,
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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. 99974-66-0, name is Diethyl 3-hydroxycyclobutane-1,1-dicarboxylate, A new synthetic method of this compound is introduced below., name: Diethyl 3-hydroxycyclobutane-1,1-dicarboxylate

A solution of alcohol Id (3.0 g) in 200 mL of dichloromethane was treated with Dess-Martin periodinane (1.2 eq, 7.06 g). The mixture was stirred for 2 h at room temp. The reaction was quenched by addition of aq saturated sodium thiosulfate soln (100 mL). The mixture was stirred for 20 min followed by addition of aq saturated sodium bicarbonate soln (100 mL). The mixture was further stirred for 20 min and extracted with ethyl acetate (500 mL). The aqueous layer was back extracted with ethyl acetate (250 mL). The combined organic layers were washed with aq saturated sodium bicarbonate (2 x 80 mL) and brine (80 mL). The organic layer was dried over magnesium sulfate, filtered and concentrated in rotavap. The product was purified on silica gel (Biotage75-M column; gradient: 0 to 30% ethyl acetate in hexanes) to afford the product (5.14 g; 96 %) as a colorless oil.

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; SCHERING CORPORATION; WO2009/8913; (2009); A2;,
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Related Products of 1214334-90-3, 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. 1214334-90-3, name is Methyl 2-bromo-4-(trifluoromethyl)benzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 2: 2-Cvclopropyl-4-trifluoromethyl-benzoic acid methyl esterTo a solution of 400 mg (1.413 mmol) 2-bromo-4-trifluoromethyl-benzoic acid methyl ester ,146 mg (1.696 mmol) cyclopropyl boronic acid, 1.21g (4.946 mmol) tri-potassium phosphate monohydrate, 40.9 mg (0.141 mmol) tricyclohexyl phosphine in 6 ml toluene and 0.3 ml water under nitrogen at room temperature, was added 15.9 mg (0.0707 mmol) palladium acetate. The mixture was stirred in a 100 0C oil bath for 4 hours and overnight at room temperature under nitrogen. The mixture was cooled to room temperature. Water was added and the mixture extracted with ethyl acetate. The organic layer was washed once with brine, dried over sodium sulfate, filtered and concentrated in vacuo. The crude compound was purified on silica gel (eluent: heptane/ethyl acetate 0 to 10 %) to provide 0.24 g (71 %) of the title compound as a yellow oil.

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-bromo-4-(trifluoromethyl)benzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; KOLCZEWSKI, Sabine; PINARD, Emmanuel; WO2011/23667; (2011); A1;,
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Adding a certain compound to certain chemical reactions, such as: 26759-46-6, name is Methyl 2-amino-4,5-dimethoxybenzoate, 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 26759-46-6, Computed Properties of C10H13NO4

Example 1: (Production of 6,7-dimethoxyquinazolin-4-one); Using acetic acid and an inorganic base, ammonia, as a catalyst, 6,7-dimethoxyquinazolin-4-one was produced in the manner mentioned below. 0.84 g (4 mmol) of methyl 4,5-dimethoxyanthranilate, 3.60 g (80 mmol) of formamide, 0.17 g (2.8 mmol) of acetic acid and 0.05 g (2.8 mmol) of ammonia from a pressure cylinder were put into an autoclave of SUS316 having a capacity of 25 mL and equipped with a stirrer, a thermometer and a pressure gauge in a nitrogen atmosphere, and reacted at 150C for 2 hours. After the reaction, the reaction liquid was cooled to room temperature, and the precipitated crystal was collected by filtration, washed with methanol and then dried in vacuum at 70C for 2 hours to obtain 0.77 g of a crystal. The obtained crystal was analyzed for the purity by high-performance liquid chromatography, and its purity was 99.5 %; and 6,7-dimethoxyquinazolin-4-one was obtained at a yield of 93.0 %. The result is shown in Table 1. Examples 2 to 4, and Comparative Examples 1 and 2: (Production of 6,7-dimethoxyquinazolin-4-one); The reaction and the post-treatment were carried out in the same manner as in Example 1, for which, however, the catalyst was changed as in Table 2. In Example 4, ammonium acetate was used as the catalyst; and in Comparative Examples 1 and 2, formic acid or potassium carbonate, respectively, was used alone as the catalyst like in JP-A 2002-338550 (Patent Reference 4). From the results in Table 1, it is known that the reaction system with acetic acid and a base coexisting therein of the present invention gives 6,7-dimethoxyquinazolin-4-one at a higher yield than the conventional reaction system with formic acid or potassium carbonate alone therein.

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; Mitsubishi Gas Chemical Company, Inc.; EP1997812; (2008); A1;,
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