(S)-2-羟基-3-甲氧基-3,3-二苯基丙酸合成路线 (共 10 条)
反应条件
(S)-(-)-α-methyl-4-nitro-benzylamine in tert-butyl methyl ether; acetone T=10 - 55°C; 13 h; Resolution of racemate;
参考文献
NATCO PHARMA LIMITED; KOMPELLA, Amala; ADIBHATLA, Kali Satya Bhujanga Rao; BALINA, Veera Swamy; KASA, Srinivasu; NANNAPANENI, Venkaiah Chowdary
Patent: WO2012/17441 A1, 2012 ;
Location in patent: Page/Page column 11-12 ;
反应条件
1.1: sodium methylate / tetrahydrofuran / 2 h / -10 - -4 °C 1.2: 2.75 h / 0 - 35 °C 2.1: sodium hydroxide; water / 2 h / 95 - 100 °C 2.2: 40 - 45 °C / pH 1.3 3.1: sodium methylate; (S)-2-carbomethoxypyrrolidine hydrochloride / tert-butyl methyl ether; methanol / 1.25 h / 25 - 60 °C / Reflux View Scheme
参考文献
US2011/263854 A1, ;
US 20110263854 A1
反应条件
1.1: sodium hydroxide; water / 2 h / 95 - 100 °C 1.2: 40 - 45 °C / pH 1.3 2.1: sodium methylate; (S)-2-carbomethoxypyrrolidine hydrochloride / tert-butyl methyl ether; methanol / 1.25 h / 25 - 60 °C / Reflux View Scheme
参考文献
US2011/263854 A1, ;
US 20110263854 A1
反应条件
1.1: 0.25 h 1.2: 0.04 h / 20 - 55 °C 2.1: sodium hydroxide; water / 1.5 h / 90 - 95 °C 3.1: (S)-(-)-α-methyl-4-nitro-benzylamine / tert-butyl methyl ether; acetone / 13 h / 10 - 55 °C / Resolution of racemate View Scheme
反应条件
1.1: toluene-4-sulfonic acid / 48 h / 25 - 35 °C 2.1: potassium carbonate / acetone / 0.67 h / 25 - 35 °C 2.2: 10 h / 55 - 60 °C 3.1: sodium hydroxide / water; methanol / 3 h / 25 - 60 °C 3.2: pH 5.8 View Scheme
参考文献
CIPLA LIMITED; KING, Lawrence; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; NAIK, Sanjay; GHAGARE, Maruti; CHIKHALIKAR, Sandip Vasant
Patent: WO2013/57468 A1, 2013 ;
反应条件
sodium methylate in N,N-dimethyl-formamide T=5 - 28°C; Inert atmosphere;
参考文献
CIPLA LIMITED; KING, Lawrence; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; NAIK, Sanjay; GHAGARE, Maruti; CHIKHALIKAR, Sandip Vasant
Patent: WO2013/57468 A1, 2013 ;
Location in patent: Page/Page column 25 ;
反应条件
1: With potassium carbonate in N,N-dimethyl-formamide T=20 - 25°C; 3 h; Large scale; 2: With dimethyl sulfate in N,N-dimethyl-formamide T=20 - 25°C; 3 h; Large scale;
参考文献
Jansen; Knopp; Amberg; Bernard; Koser; Mueller; Muenster; Pfeiffer; Riechers
Organic Process Research and Development, 2001 , vol. 5, # 1 p. 16 - 22
反应条件
hydrogenchloride T=25 - 35°C; 48 h;
参考文献
Reddy, Manne Satyanarayana; Nagaraju, Chakilam; Ramprasad, Achampeta Kodanda
Patent: US2011/263854 A1, 2011 ;
Location in patent: Page/Page column 8 ;
US 20110263854 A1
反应条件
Lactobacillus paracasei DSM 20207 in water T=42°C; pH=6; 24 h; Product distribution; Further Variations:Reagents;
参考文献
Nestl, Bettina M.; Glueck, Silvia M.; Hall, Melanie; Kroutil, Wolfgang; Stuermer, Rainer; Hauer, Bernhard; Faber, Kurt
European Journal of Organic Chemistry, 2006 , # 20 p. 4573 - 4577
反应条件
1.1: toluene-4-sulfonic acid / 48 h / 25 - 35 °C
2.1: potassium carbonate / N,N-dimethyl-formamide / 0.67 h / 25 - 35 °C
2.2: 4 h / 90 - 95 °C
View Scheme
参考文献
CIPLA LIMITED; KING, Lawrence; RAO, Dharmaraj Ramachandra; KANKAN, Rajendra Narayanrao; NAIK, Sanjay; GHAGARE, Maruti; CHIKHALIKAR, Sandip Vasant
Patent: WO2013/57468 A1, 2013 ;