137973-76-3
137973-76-3 結(jié)構(gòu)式
基本信息
托伐普坦雜質(zhì)5(DM-21826)
7-氯-1-[2-甲基-4-[(2-甲基苯甲酰)氨基]苯甲酰
N-(4-(7-氯-5-氧代-2,3,4,5-四氫-1H-苯并[B]氮雜-1-羰基)-3-甲基苯基)-2-甲基苯甲酰胺
7-氯-1-[2-甲基-4-[(2-甲基苯甲酰)氨基]苯甲?；鵠-5-氧代-2,3,4,5-四氫-1H-1-苯并氮雜卓
N-(4-(7-氯-5-氧代-2,3,4,5-四氫-1H-苯并[B]氮雜卓-1-羰基)-3-甲基苯基)-2-甲基苯甲酰胺
N-[4-[(7-氯-2,3,4,5-四氫-5-氧代-1H-1-苯并氮雜卓-1-基)羰基]-3-甲基苯基]-2-甲基苯甲酰胺
N-[4-[(7-氯-2,3,4,5-四氫-5-氧代-1H-1-苯并氮雜卓-1-基)羰基]-3-甲基苯基]-2-甲基苯甲酰胺
N-[4-[(7-CHLORO-2,3,4,5-TETRAHYDRO-5-OXO-1H-1-BENZAZEPIN-1-YL)CARBONYL]-3-METHYLPHENYL]-2-METHYLBENZAMIDE CAS號(hào):137973-76-3
N-[4-[(7-Chloro-2,3,4,5-tetrahydro-5-oxo-1H-1-benzazepin-1-yl)carbonyl]-3-methylphenyl]-2-methylbenzamide CAS號(hào): 137973-76-3
5-Dehydro Tolvaptan
Tolvaptan Intermediate
Tolvaptan 5-Oxo Analog
Tolvaptan impurity 5 (DM-21826)
7-chloro-1-[2-methyl-4-[(2-methylbenzoyl)amino]benzoyl]-5-ox...
N-(4-(7-Chloro-5-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepine-1-carbonyl)-3-methylphenyl)-2-methy
N-[4-(7-chloro-5-oxo-3,4-dihydro-2H-1-benzazepine-1-carbonyl)-3-methylphenyl]-2-methylbenzamide
N-(4-(7-Chloro-5-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepine-1-carbonyl)-3-methylphenyl)-2-methylbe
7-chloro-1-[2-methyl-4-[(2-methylbenzoyl)amino]benzoyl]-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine
物理化學(xué)性質(zhì)
制備方法
933-88-0
137977-97-0
137973-76-3
向3 L反應(yīng)釜中加入1-(4-氨基-2-甲基苯甲?；?-7-氯-3,4-二氫-1H-苯并[b]氮雜卓-5(2H)-酮（70.0 g，212.90 mmol）、二氯甲烷（560 mL）和蒸餾水（140 mL），攪拌反應(yīng)混合物1小時(shí)。在溫度控制在10℃以下的條件下，向反應(yīng)混合物中緩慢加入氫氧化鎂（14.90 g，14.90 mmol），繼續(xù)攪拌30分鐘。隨后，緩慢滴加鄰甲基苯甲酰氯（30.42 mL），滴加完畢后繼續(xù)攪拌反應(yīng)3小時(shí)。反應(yīng)完成后，過濾除去氫氧化鎂，用氫氧化鈉水溶液調(diào)節(jié)濾液的pH至8-9，分離有機(jī)層。有機(jī)層用無水硫酸鈉干燥，過濾后減壓濃縮，得到7-氯-1-[2-甲基-4-[(2-甲基苯甲酰)氨基]苯甲?；鵠-5-氧代-2,3,4,5-四氫-1H-1-苯并氮雜卓91.35 g，產(chǎn)率為96%。
參考文獻(xiàn)：
[1] Patent: JP2018/12690, 2018, A. Location in patent: Paragraph 0029; 0030
[2] Patent: CN105315169, 2016, A. Location in patent: Paragraph 0170; 0224; 0225
[3] Patent: CN105753735, 2016, A. Location in patent: Paragraph 0181; 0217; 0218
[4] Patent: CN106883175, 2017, A. Location in patent: Paragraph 0017; 0018
[5] Patent: CN108503586, 2018, A. Location in patent: Paragraph 0044; 0045; 0054; 0055; 0056