(2S,4E)-5-氯-N,N-二甲基-2-异丙基-4-戊烯酰胺合成路线 （共 11 条）
反应条件
pyridine in dichloromethane T=-10 - 0°C; 2 h;
参考文献
Speedel Pharma AG
Patent: EP1200384 B1, 2004 ;
Location in patent: Page 8 ;
反应条件
1: With isopropylmagnesium chloride in tetrahydrofuran T=30 - 35°C; Inert atmosphere; 2: With hydrogenchloride; ammonium chloride in tetrahydrofuran; water
参考文献
DR. REDDY'S LABORATORIES LTD.; DR. REDDY'S LABORATORIES, INC.; KOLLA, Naveen Kumar; APPAYE, Kaliyaperumal Srinivasan; GANGULA, Srinivas; GOVINDAPUR, Rajeshwar Reddy; MANNE, Nagaraju; NIKUMBH, Satish Pandurang; NEELAM, Uday Kumar; JOSEPH, Suju Chuttippari; BADDAM, Sudhakar Reddy; KUNHIMON, Shyam Kumar Unniaranpurakkal; MOOVENDAN, Mohan; DAHANUKAR, Vilas; DONIPARTHI, Kiran Kumar
Patent: WO2012/21446 A2, 2012 ;
Location in patent: Page/Page column 35 ;
反应条件
1: dimethyl amine With trimethylaluminum in toluene T=-15 - 0°C; 1 h; 2: (S,E)-ethyl 5-chloro-2-isopropylpent-4-enoate in toluene T=80°C; 22 h; 3: With hydrogenchloride; water in toluene
参考文献
Speedel Pharma AG
Patent: EP1200384 B1, 2004 ;
Location in patent: Page 8; 9 ;
反应条件
1: potassium carbonate / N-benzyl-N,N,N-triethylammonium chloride / acetonitrile / 12 h / 50 - 55 °C 2: methanol / 12 h / Reflux 3: sodium hydroxide / Esterase V enzime / 24 h / pH ~ 10 / Sodium carbonate buffer; Resolution of racemate; Enzymatic reaction 4: isopropylmagnesium chloride / tetrahydrofuran / 30 - 35 °C / Inert atmosphere View Scheme
反应条件
1.1: potassium hydroxide / 2-methoxy-ethanol / 3 h / 120 °C 1.2: pH 2 1.3: 65 °C 2.1: sodium hydroxide / Esterase V enzime / 24 h / pH ~ 10 / Sodium carbonate buffer; Resolution of racemate; Enzymatic reaction 3.1: isopropylmagnesium chloride / tetrahydrofuran / 30 - 35 °C / Inert atmosphere View Scheme
反应条件
1.1: potassium hydroxide / tetrabutylammomium bromide / toluene / 0.17 h 1.2: 4 h / 30 - 35 °C 2.1: potassium hydroxide / 2-methoxy-ethanol / 3 h / 120 °C 2.2: pH 2 2.3: 65 °C 3.1: sodium hydroxide / Esterase V enzime / 24 h / pH ~ 10 / Sodium carbonate buffer; Resolution of racemate; Enzymatic reaction 4.1: isopropylmagnesium chloride / tetrahydrofuran / 30 - 35 °C / Inert atmosphere View Scheme
反应条件
1: sodium hydroxide / Esterase V enzime / 24 h / pH ~ 10 / Sodium carbonate buffer; Resolution of racemate; Enzymatic reaction 2: isopropylmagnesium chloride / tetrahydrofuran / 30 - 35 °C / Inert atmosphere View Scheme
反应条件
1: methanol / 12 h / Reflux 2: sodium hydroxide / Esterase V enzime / 24 h / pH ~ 10 / Sodium carbonate buffer; Resolution of racemate; Enzymatic reaction 3: isopropylmagnesium chloride / tetrahydrofuran / 30 - 35 °C / Inert atmosphere View Scheme
反应条件
1.1: magnesium; ethylene dibromide / 2-methyl tetrahydrofuran / 60 - 65 °C 1.2: 0.25 h / 10 °C 2.1: N-bromosuccinmide; phosphoric acid / water; tetrahydrofuran / 5 °C 3.1: sodium azide; Aliquatreg; 336 / water / 48 h / 75 - 80 °C View Scheme
反应条件
1.1: magnesium; ethylene dibromide / tetrahydrofuran / 4.17 h / 63 - 68 °C / Inert atmosphere 1.2: 1 h / 0 - 5 °C 2.1: N-bromosuccinmide; phosphoric acid / water; tetrahydrofuran / 1.25 h / 0 - 5 °C 3.1: sodium azide / ethylene glycol / 20 h / 80 - 85 °C 4.1: triethylamine; 2-hydroxy-pyridine / 16 h / 85 - 90 °C 5.1: hydrogen; ethanolamine / palladium 10 on activated carbon / isopropyl alcohol / 3 h View Scheme
