Month: June 2021

Electric Literature of 27492-84-8, The chemical industry reduces the impact on the environment during synthesis 27492-84-8, name is Methyl 4-amino-2-methoxybenzoate, I believe this compound will play a more active role in future production and life.

Iodine monochloride (0.54mL, 10.5mmol)Add to methyl 4-amino-2-methoxybenzoate (1.8 g, 10 mmol)Stirring was continued for 1 hour in the methanol solution. The reaction solution is poured into water,Extracted with ethyl acetate (3×50 mL), washed with saturated brineFilter, spin dry petroleum ether / ethyl acetate (3/1)The compound 68D (2.7 g, 90percent yield) was isolated and purified.

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-2-methoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangsu Xiansheng Pharmaceutical Co., Ltd.; Chen Huanming; Liang Bo; Cao Wenjie; Zhang Guiping; Zhao Zhongqiang; Jiang Zhaojian; Zuo Gaolei; Xu Wanmei; Gong Hongju; Zhang Peng; Wang Jianghuai; Li Qingsong; Gao Chunhua; (79 pag.)CN104045552; (2019); B;,
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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. 884497-46-5, name is Methyl 3-amino-5-fluorobenzoate, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H8FNO2

General procedure: To a solution of compound 11a (154 mg, 1.0 mmol) in anhydrous CH2Cl2 (10 mL) was added 3,5-dichlorobenzoyl chloride (209 mg, 1.0 mmol) and pyridine (241 mL 3.0 mmol) under ice bath. After stirring at room temperature for about 8 h, the solvent was removed in vacuum. The resulting residue was dissolved in NaOH (1 M) water solution (3 mL) and CH3OH (3 mL) and stirred for another 2 h. Then the solvent was removed under vacuum, and the residue was acidied to pH 2 or below with HCl (1 M) water solution. The solution was extracted with ethyl acetate twice and the combined organics were dried over anhydrous sodium sulfate and concentrated in vacuum. The resulting residue was puried by silica gel chromatography to give the desired compound as a white solid (234 mg, yield 85.0%)

The synthetic route of 884497-46-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gao, Ding-Ding; Dou, Hui-Xia; Su, Hai-Xia; Zhang, Ming-Ming; Wang, Ting; Liu, Qiu-Feng; Cai, Hai-Yan; Ding, Hai-Peng; Yang, Zhuo; Zhu, Wei-Liang; Xu, Ye-Chun; Wang, He-Yao; Li, Ying-Xia; European Journal of Medicinal Chemistry; vol. 154; (2018); p. 44 – 59;,
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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. 35120-18-4, name is Ethyl 1-bromocyclobutanecarboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: Ethyl 1-bromocyclobutanecarboxylate

General procedure: A mixture of thiones or thiol 5a-5q or 5ha-5hi (60 mmol), bromoacetates BrCH2CO2Me,(CH3)2CBrCO2Et or ethyl 1-bromocyclobutanecarboxylate (80 mmol) and K2CO3 (16.59 g, 120 mmol)in a suitable solvent (200 mL; acetone for 5a-5b or DMF for the others) was stirred at a temperaturespecified in Schemes 1-5 until the completion of reaction as indicated by TLC analysis (typicallywithin 12 h). On cooling to room temperature (if necessary), for 5a-5b: the reaction mixture wasfiltered off and the filtrate was evaporated on a rotary evaporator to give a residue, which waspurified by column chromatography to afford 6a-6b; for the others: the reaction mixture was pouredinto ice-water (300 mL), and the resulting mixture was extracted with CH2Cl2 (100 mL × 3). Thecombined extracts were washed with 5% brine (100 mL × 5), dried (Na2SO4) and evaporated on arotary evaporator to afford the crude product as a residue, which was purified by columnchromatography to yield the pure product 6c-6x or 6ha-6hi.

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:
Article; Cai, Wenqing; Wu, Jingwei; Liu, Wei; Xie, Yafei; Liu, Yuqiang; Zhang, Shuo; Xu, Weiren; Tang, Lida; Wang, Jianwu; Zhao, Guilong; Molecules; vol. 23; 2; (2018);,
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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. 3044-06-2, name is Diethyl 2-(1-ethoxyethylidene)malonate, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C11H18O5

In a round-bottom flask, equipped with a stirrer, thermometer and reflux condenser, mix under nitrogen in the specified order: 1 g (0.0048 mol) of BCD-BTK-13-14 and 1.18 g (0.0051 mol) of diethyl-2-(1- ethoxyethylidene)malonate. Heat the mixture for 2 hours at 125-130 . Distill off the residual solvent using a rotary evaporator. Take the mixture to the next step without additional purification. Yield: 1.88 g (99%).

According to the analysis of related databases, 3044-06-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JOINT STOCK COMPANY “BIOCAD”; GAVRILOV, Aleksey Sergeevich; ALESHUNIN, Pavel Aleksandrovich; GORBUNOVA, Svetlana Leonidovna; REKHARSKY, Mikhail Vladimirovich; KOZHEMYAKINA, Natalia Vladimirovna; KUKUSHKINA, Anna Aleksandrovna; KUSHAKOVA, Anna Sergeevna; MIKHAYLOV, Leonid Evgen`evich; MOLDAVSKY, Alexander; POPKOVA, Aleksandra Vladimirovna; SILONOV, Sergey Aleksandrovich; SMIRNOVA, Svetlana Sergeevna; IAKOVLEV, Pavel Andreevich; (197 pag.)WO2018/92047; (2018); A1;,
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Application of 369-26-6, 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. 369-26-6, name is Methyl 3-amino-4-fluorobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

A mixture solution of 3-amino-4-fluoro-benzoic acid methyl ester (26 g, 153.8 mmol), 3-bromo-benzaldehyde (28.5 g, 153.8 mmol) and p-toluenesulfonic acid (590 mg, 3.2 mmol) in toluene (200 mL) was heated to reflux for 12 hours. Then the reaction mixture was cooled to room temperature. The solvent was removed in vacuo and the residue was washed with ether to afford 3-[(3-bromo-benzylidene)-amino]-4-fluoro-benzoic acid methyl ester (51.7 g, quant.) as a pale-white solid: MS calcd. for C15H11BrFlNO2 337.16, obsd. (ESI+) [(M+H)+] 336.0 338.0

The chemical industry reduces the impact on the environment during synthesis Methyl 3-amino-4-fluorobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Chen, Li; Feng, Lichun; Huang, Mengwei; Liu, Yongfu; Wu, Guolong; Wu, Jim Zhen; Zhou, Mingwei; US2011/257151; (2011); A1;,
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Electric Literature of 99548-54-6, A common heterocyclic compound, 99548-54-6, name is Methyl 3-bromo-2-methylbenzoate, molecular formula is C9H9BrO2, 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 flask was added methyl 3-bromo-2-methylbenzoate (21 g, 91.7 mmol), potassium hexacyanoferrate (II) trihydrate (9.7 g, 22.9 mmol), Na2CO3 (9.7 g, 91.7 mmol) and Pd(OAc)2 (102 mg) in N,N-dimethylacetamide (100 mL). The flask’s atmosphere was evacuated and replaced with nitrogen, and the reaction mixture heated at 120 C. for 10 hours. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (150 mL). The resultant slurry was filtered and washed thoroughly with ethyl acetate (2×50 mL). The combined filtrate was washed with brine and water, dried over Na2SO4 and evaporated under reduced pressure. The residue obtained after the concentration was purified using flash chromatography (ethyl acetate-hexanes (1:9) as the eluent) to provide methyl 3-cyano-2-methylbenzoate (11.2 g, 70% yield). 1H NMR spectrum (in DMSO-d6): delta 8.03 (d, J=8.1 Hz, 1H); 7.98 (d, J=7.9 Hz, 1H); 7.49 (t, 1H); 3.84 (s, 3H); 2.65 (s, 3H).

The synthetic route of 99548-54-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Inotek Pharmaceuticals Corporation; US2007/49555; (2007); A1;,
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Adding a certain compound to certain chemical reactions, such as: 3618-04-0, name is trans-Ethyl 4-hydroxycyclohexanecarboxylate, 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 3618-04-0, HPLC of Formula: C9H16O3

tert-Butyldimethylsilyl chloride (26.3 g, hydroxycyclohexanecarboxylate (25.0 g, 171 59-80-7) and imidazole (24.7 g, 363174 mmol) was added to a solution of ethyl 4-145 mmol, mixture of cis-/trans-isomers, Gas Nommol) in N,N-dimethylformamide (36 ml) and the mixture was stirred over night at room temperature. For work-up, water was added and the mixture was extracted with tert-butyl methyl ether (3x). The combined organic phases were washed with brine, filtrated through a silicone filter and concentrated under reduced pressure to yield ethyl 4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexanecarboxylate (43.1 g, 104% yield) which was used in the next step without further purification. 1HNMR (400 MHz, DMSO-d6, mixture of isomers): 6 [ppm] = 4.10-3.99 (m, 2H), 3.93-3.86 (m, 0.7H), 3.63-3.51 (m, 0.3H), 2.39-2.28 (m, 0.8H), 2.27-2.14 (m, 0.3H), 1.91-1.21 (m, 8H), 1.20-1.13 (m, 3H), 0.89-0.79 (m, 9H), 0.08-0.00 (m, 6H).

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, trans-Ethyl 4-hydroxycyclohexanecarboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; EIS, Knut; ACKERMANN, Jens; WAGNER, Sarah; BUCHGRABER, Philipp; SUeLZLE, Detlev; HOLTON, Simon; BENDER, Eckhard; LI, Volkhart; LIU, Ningshu; SIEGEL, Franziska; LIENAU, Philip; BAIRLEIN, Michaela; VON NUSSBAUM, Franz; HERBERT,Simon; KOPPITZ, Marcus; (734 pag.)WO2016/177658; (2016); A1;,
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These common heterocyclic compound, 53518-15-3, name is 7-Amino-4-(trifluoromethyl)-2H-chromen-2-one, 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. HPLC of Formula: C10H6F3NO2

To a solution of 2 (1.40g, 6.11mmol), in 20mL CH2Cl2 was added triethylamine (1.78mL, 12.81mmol) and the solution was stirred at 35C for 20min. After cooling the system to room temperature, thiophosgene (1.40mL, 18.37mmol) was added dropwise and the mixture was stirred at 35C for 20min. The reaction was completed after 20min, as indicated by TLC (Hexanes:EtOAc=8:1). Excess of CSCl2 was removed by distillation in high vacuum. The orange precipitate was dissolved in 20mL CH2Cl2, filtered through silica gel for the removal of triethylamine hydrochloride, washed with 10mL dichloromethane, and dried in high vacuum to yield 1.37g (83.0%) of product as a light orange solid.mp: 119.7-120.8C. 1H NMR (300MHz, DMSO-d6): delta (ppm)=7.73-7.76 (m, 1H, ArH), 7.71 (d, 1H, J=2.1Hz, ArH), 7.50 (dd, 1H, J1=2.1Hz, J2=8.7Hz, ArH), 7.12 (s, 1H, C-CH-C=O). 13C NMR (75MHz, DMSO-d6) delta (ppm): 158.45, 154.83, 139.03, 138.59, 136.87, 134.37, 126.56, 123.65, 118.29, 115.13, 113.00. 19F NMR (282MHz, DMSO-d6) delta (ppm): -63.42. HR-ESI-MS (C11H4F3NO2S): m/z calcd for [M+H]+=271.9993, found=271.9987.

The synthetic route of 7-Amino-4-(trifluoromethyl)-2H-chromen-2-one has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Zheng-Yi; Su, Hong-Kui; Tong, Hong-Xiao; Yin, Yue; Xiao, Tangxin; Sun, Xiao-Qiang; Jiang, Juli; Wang, Leyong; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 200; (2018); p. 307 – 312;,
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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. 1117-71-1, name is Methyl 4-bromobut-2-enoate, This compound has unique chemical properties. The synthetic route is as follows., Formula: C5H7BrO2

The (E) -4- bromo crotonate 6g (33.5mmol) was dissolved in THF (60ml) cooled to to 0 ,Under the protection of N2 was added dropwise lithium hydroxide monohydrate 1.83g (43.6mmol) in water(20mL). After the dropping 15min, 0 kept stirred 3h. And then cold water 150ml200ml of petroleum ether was added to the system to continue stirring 10min at 0 . Separating the aqueous phase, at 0 PH adjusted with concentrated hydrochloric acid to 1, with dichloromethane (80mlx3) and extracted. The combined organicPhase was dried over anhydrous sodium sulfate and concentrated to give compound X, a yellow solid 4.5g, 82% yield.In the E-4- mixed with X-bromo crotonic acid and a drop of DMF in DCM (3ml) was added dropwise a solution of oxalylChlorine (0.025g, 1.96mmol). After the dropwise addition, stirring was raised to room temperature for 1h. Completion of the reaction,The solvent was concentrated to afford the intermediate (E) -4- bromo-2-enoyl chloride III, without further treatment,It was used directly in the next reaction.

According to the analysis of related databases, 1117-71-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chengdu Zepletech Biological Pharmaceutical Co., Ltd.; Wang, Kangmin; Chen, Wei; Zhao, Gang; Liu, Jifeng; Pu, Lin; (22 pag.)CN105669521; (2016); A;,
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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. 122-63-4, name is Benzyl propionate, A new synthetic method of this compound is introduced below., Computed Properties of C10H12O2

Carbapenem Intermediate (CPI) was prepared according to the synthetic scheme shown in Scheme 1. In the first step of the process, benzyl propionate is reacted with isobutoxycarbonyloxy acetic acid methyl ester in a solvent at low temperature in the presence of LDA to form ketoester A. The ketoester A is then contacted with the acetoxyazetidinone B (prepared by any number of known, synthetic routes) in a solvent, and sodium carbonate is added. The reaction ages for a period of time at a temperature such that the reaction goes substantially to completion, generating the target lactam C.

The synthetic route of 122-63-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FOB SYNTHESIS; CHOI, Woo-Baeg; KIM, Deog-Il; GRUSZECKA-KOWALIK, Ewa; JOO, Hyung-Yeul; LIU, Shuangpei; MAO, Shuli; LI, Yongfeng; WO2011/160020; (2011); A2;,
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