2-[(2E)-3-氯-2-丙烯-1-基]-2-(1-甲基乙基)丙二酸 1,3-二甲酯合成路线 (共 5 条)
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
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 ;
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 View Scheme
反应条件
1: methyl 2-carbomethoxy-3-methylbutyrate With potassium hydroxide; tetrabutylammomium bromide in toluene
0.166667 h;
2: trans-3-chloroacrylyl chloride in toluene
T=30 - 35°C; 4 h; Product distribution / selectivity;
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 32-33 ;
反应条件
1: With calcium chloride in methanol; N,N-dimethyl-formamide
T=140 - 145°C; 12 h;
2: With hydrogenchloride; water in tert-butyl methyl ether
3: With sodium hydroxide; sulfuric acid; water
Product distribution / selectivity; more than 3 stages;
参考文献
DSM FINE CHEMICALS AUSTRIA NFG GMBH and CO KG
Patent: WO2007/17018 A1, 2007 ;
Location in patent: Page/Page column 8-9 ;
反应条件
1: With methanol; lithium chloride in N,N-dimethyl-formamide
T=140 - 142°C; 8 h;
2: With hydrogenchloride; water in tert-butyl methyl ether
Product distribution / selectivity;
参考文献
DSM FINE CHEMICALS AUSTRIA NFG GMBH and CO KG
Patent: WO2007/17018 A1, 2007 ;
Location in patent: Page/Page column 7-8 ;