3-(叔丁基二甲基硅氧基)戊二酸酐合成路线 (共 13 条)
反应条件
1.1: n-butyllithium; triphenylemethane; N-pyrrolidinylnorephedrine / toluene; hexane; tetrahydrofuran / 2 h / -78 °C 1.2: 3 h 2.1: hydrogen / palladium 10 on activated carbon / ethyl acetate 3.1: sodium methylate / 3 h / 0 - 5 °C / Cooling with ice 3.3: pH 6.5 4.1: triethylamine / hexane / 3 h / -40 °C 5.1: n-butyllithium / hexane; tetrahydrofuran / 1 h / 0 °C 5.2: 3 h / -78 °C View Scheme
参考文献
MATRIX LABORATORIES LTD.; SETHI, Madhuresh, Kumar; MAHAJAN, Sanjay; RAWAT, Vijendra, Singh; MARA, Bhairaiah; VEERA, Upendra, Nath; DATTA, Debashish
Patent: WO2011/141934 A1, 2011 ;
反应条件
1: With (9S)-6'-methoxycinchonan-9-ol in dichloromethane
T=-40 - -35°C; 15 - 20 h;
2: With hydrogenchloride in tert-butyl methyl ether; water
pH=4 - 5; Product distribution / selectivity;
参考文献
TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.
Patent: WO2008/130638 A2, 2008 ;
Location in patent: Page/Page column 31 ;
反应条件
1: BuLi / tetrahydrofuran; hexane
2: H2 / Pd(OH)2/C / ethyl acetate / Ambient temperature
3: NaOMe
View Scheme
参考文献
Karanewsky, Donald S.; Malley, Mary F.; Gougoutas, Jack Z.
Journal of Organic Chemistry, 1991 , vol. 56, # 11 p. 3744 - 3747