Month: June 2021

Related Products of 1234616-21-7,Some common heterocyclic compound, 1234616-21-7, name is Methyl imidazo[1,2-b]pyridazine-6-carboxylate, molecular formula is C8H7N3O2, 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.

Synthesis of imidazo[l,2-b]pyridazin-6-ylmethanol:To a stirred solution of imidazo[l,2-b]pyridazine-6-carboxylate (3.5 g, 22.77 mmol) in MeOH:THF (45 mL, 1 :2) was added NaBH4 (1.72 g, 45.26 mmol) portion wise at 0C and stirred for 2h. After full consumption of starting material by TLC, the reaction was diluted with saturated Na2C03 solution and extracted with EtOAc. The combined organic layer was dried over sodium sulphate, filtered and concentrated in vacuo to obtain the crude product. The crude material was washed with 50%> EtOAc/Hexane to afford crude imidazo[l,2-b]pyridazin-6-ylmethanol (2.5 g). 1H-NMR (DMSO-d6, 400 MHz): delta 8.21 (s, 1H), 8.06 (d, 1H), 7.21 (s, 1H), 7.24 (d, 1H), 5.68 (br s, 1H), 4.59 (s, 2H); LC-MS: 85.80%; 149.6 (M++l) (column; X-Select C-18, (50×3.0 mm, 3.5mu); RT 0.72 min. 5mM NH4OAc in water: ACN; 0.8 ml/min); TLC: 100% EtOAc (Rf: 0.2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl imidazo[1,2-b]pyridazine-6-carboxylate, its application will become more common.

Reference:
Patent; ENVIVO PHARMACEUTICALS, INC.; RIPKA, Amy; SHAPIRO, Gideon; MCRINER, Andrew; WO2012/40230; (2012); A1;,
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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. 431-47-0, name is Methyl 2,2,2-trifluoroacetate, A new synthetic method of this compound is introduced below., Application In Synthesis of Methyl 2,2,2-trifluoroacetate

Compound 24 (2.127 g, 3.6 mmol) was dissolved in DCM (10 g), and treated with triethylamine (0.1 mL) and methyltrifluoroacetate (0.922 g, 7.2 mmol) at 30 C. for 4 h. The reaction mixture was evaporated and purified on a silica gel column (50% hexanes/DCM?4% MeOH/DCM) to give compound 8b (1.914 g, 77.4%).

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; AM Chemicals LLC; GUZAEV, Andrei Pavel; VVEDENSKIY, Vladimir V.; GOGOI, Khirud; (90 pag.)US2018/16232; (2018); A1;,
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Related Products of 185312-82-7, 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. 185312-82-7, name is Methyl 4-bromo-2-chlorobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

At 0C, lithium aluminum hydride (1.09 g, 30 mmol) was dropped into a solution of methyl 4-bromo-2-chlorobenzoate (4.78 g, 19.16 mmol) in tetrahydrofuran (100 mL) slowly. The ice-salt bath used was removed after that dropping. The reaction was complete (detected with LCMS and TLC) after stirred for 1 hour at room temperature. The mixture was cooled to 0C again and the reaction was quenched with water (1.09 mL) and 10% NaOH solution (10.9 mL) respectively. After stirred for 15 min at room temperature, the mixture was filtered and then the filter cake was washed with tetrahydrofuran (50 mLx2) and ethyl acetate EA (50 mLx2). The filtrate was dried with anhydrous sodium sulfate, filtered, and then concentrated to obtain a colorless oil product (3.4 g, 80% yield). The molecular ion peak shown by liquid chromatography-mass spectrometry was: MS (ESI): m/z 202.9/204.9 [M-OH]+.

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

Reference:
Patent; SUZHOU CONNECT BIOPHARMACEUTICALS, LTD.; ZHENG, Wei; PAN, Wubin; YANG, Xin; (47 pag.)EP3048103; (2016); A1;,
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Related Products of 13671-00-6, 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. 13671-00-6, name is Methyl 2,6-difluorobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

a) Methyl 2-JZUORO-6-PHENOXYBENZOATE Methyl 2,6-difluorobenzoate (2 g), phenol (1.09 g), caesium carbonate (3.79 g), and dimethylformamide (10 mL) were loaded in a 100 mL round bottom flask and the resulting suspension heated to 80C for 6 h. After cooling the reaction to room temperature, water (30 mL) was added and the mixture extracted with dichloromethane (2 x 30 mL). The combined organic extracts were washed with brine (30 mL), dried (magnesium sulphate), filtered and evaporated in vacuo. The residue was purified by column chromatography (Silica: DICHLOROMETHANE/HEXANE 5: 2) to give the titled compound as a clear oil (1.7 g)

The chemical industry reduces the impact on the environment during synthesis Methyl 2,6-difluorobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ASTRAZENECA AB; WO2004/113303; (2004); 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. 56741-34-5, name is Methyl 5-amino-2-fluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of Methyl 5-amino-2-fluorobenzoate

General procedure: To a solution of 11a (500 mg, 1.85 mmol) in acetone (10 mL) was added 12 (380 mg, 1.85 mmol) and pyridine (0.45 mL, 5.54 mmol).The mixture was stirred at 55 C for 1 h. The mixture was concentrated,diluted with ethyl acetate and washed with 1M HCl and brine twice.Then, the ethyl acetate layer was dried over anhydrous sodium sulfate andconcentrated to give the crude product. The crude product was purified bysilica column eluting with petroleum ether/ethyl acetate (5/1-2/1) to givethe desired product (0.33 g, yield 44.3%) as grey solid

The synthetic route of 56741-34-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; He, Yulong; Dou, Huixia; Gao, Dingding; Wang, Ting; Zhang, Mingming; Wang, Heyao; Li, Yingxia; Bioorganic and Medicinal Chemistry; vol. 27; 19; (2019);,
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Related Products of 40872-87-5,Some common heterocyclic compound, 40872-87-5, name is Methyl 3-amino-4-chlorobenzoate, molecular formula is C8H8ClNO2, 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 250 mL round bottom flask equipped with a stir bar was added 2-methylsulfanyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid (4.0 g, 17.0 mmol) (from Example 24 supra), 3-amino-4-chloro-benzoic acid methyl ester (4.6 g, 25.0 mmol), N,N-dimethylformamide (45 mL) and triethylamine (4.9 mL, 35.0 mmol), after which HATU (9.5 g, 25.0 mmol) was added all at once. The reaction was allowed to stir at room temperature for 18 hours after which the reaction was diluted with ethyl acetate and the precipitate was filtered, rinsed with water, ethyl acetate and then dried under high vacuum to provide 4-chloro-3-[(2-methylsulfanyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidine-6-carbonyl)-amino]-benzoic acid methyl ester as an off-white solid. (Yield 5.27 g, 76%).

The synthetic route of 40872-87-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anderson, Kevin; Chen, Yi; Chen, Zhi; Luk, Kin-Chun; Rossman, Pamela Loreen; Sun, Hongmao; Wovkulich, Peter Michael; US2012/184542; (2012); 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. 26218-04-2, name is 2-Ethylhexyl 4-aminobenzoate, A new synthetic method of this compound is introduced below., Product Details of 26218-04-2

Example 2Synthesis of 2, 5, 8-tris- (4- (2- ethylhexyloxycarbonyl) phenylamino) -1,3,4,6,7,9, 9b- heptaazaphenalene .A mixture of 2, 5, 8-trichloro-l, 3, 4, 6, 7, 9, 9b- heptaazaphenalene (50 mg, 0.18 mmol) and 2-ethylhexyl 4- aminobenzoate (270 mg, 1.08 mmol) in toluene (2 mL) is refluxed for 1 hour. The solvent is evaporated in vacuo and the crude product is purified by silica gel column chromatography, eluting with hexane / ethyl acetate 2 / 1. 2,5, 8-tris- (4- (2-ethylhexyloxycarbonyl) phenylamino) – 1, 3, 4, 6, 7, 9, 9b-heptaazaphenalene is obtained (160 mg, 0.17 mmol, 97%) . M. P. 183-186 C.1H NMR (300 MHz, DMSO-d6): ? 0,93 (m, 18H), 1,30 (m, 24H), 1,62 (m, 3H), 4,18 (d, J = 5.4 Hz, 6H), 7,95 (m, 12H), 10,85 (m, 3H) .MS-EI (m/z) : 916 (M+l) . UV: ?max = 326 nm; ? = 95000 M”1 cm”1 (CHCl3) .

The synthetic route of 26218-04-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ISDIN, S.A.; WO2007/6807; (2007); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 35179-98-7, 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. 35179-98-7, name is Chloromethyl ethyl carbonate, This compound has unique chemical properties. The synthetic route is as follows.

To DMF (10 mL) were added chloromethyl ethyl carbonate (0.66 g, 4.77 mmol),potassium carbonate (1.00 g, 7.16 mmol) and (2S,3S)-3-((2-bromo-6-(5-chlorothiophen-2-yl)-5-fluoropyrimidin-4-yl)amino)bicyclo[2.2.2]octane-2-carboxylic acid (1.10 g, 2.39 mmol) andthe mixture was stirred at rt overnight. To the reaction mixture was added water (40 mL), and theresulting mixture was extracted with ethyl acetate (30 mL x 3). The combined organic layerswere washed with saturated brine (30 mL), dried over anhydrous sodium sulfate and filtered. Thefiltrate was concentrated and the residue was purified by silica gel column chromatography(PE/EtOAc (v/v) = 1511) to give the title compound as a light yellow solid (0.90 g, 67 %).

The chemical industry reduces the impact on the environment during synthesis Chloromethyl ethyl carbonate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; TANG, Changhua; REN, Qingyun; YIN, Junjun; YI, Kai; LEI, Yibo; WANG, Yejun; ZHANG, Yingjun; (303 pag.)WO2018/108125; (2018); A1;,
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Some common heterocyclic compound, 46004-37-9, name is Methyl 4-amino-2-chlorobenzoate, molecular formula is C8H8ClNO2, 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. Recommanded Product: Methyl 4-amino-2-chlorobenzoate

1 g of methyl 4-amino-2-chlorobenzoate was cooled to 0C in DCM with 485 muL of Pyridine before Methanesulfonyl Chloride was added dropwise. The reaction was allowed to warm to room temperature and stir overnight. Solvent was concentrated and the crude material was dissolved in Ethyl Acetate and extracted with saturated bicarbonate solution and then brine. The crude material was dried over Magnesium Sulfate, filtered and concentrated to give 1.54 g of methyl 2-chloro-4-(methylsulfonamido)benzoate.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 46004-37-9, its application will become more common.

Reference:
Patent; GENENTECH, INC.; CURIS, INC.; WO2009/126863; (2009); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Application of 175278-29-2, 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. 175278-29-2, name is Methyl 5-fluoro-2-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows.

step 2: Compound 2 (19.5 g, 0.1 mol) was dissolved in 80 mL of acetic acid and 50 mL of acetic anhydride, and the temperature was lowered to 10 C. Potassium nitrate (15.2 g, 0.15 mol) was added in portions, and after the addition, the reaction was carried out for 6 h. The insoluble material was removed by filtration, and the reaction mixture was poured into 400 mL of ice water, filtered, and dried to give 17.3 g of Compound 3.

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

Reference:
Patent; Cheng Chunxiao; (7 pag.)CN108409626; (2018); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics