N-Boc-3-氨基丙基溴合成路线 (共 24 条)
反应条件
With sodium hydride in N,N-dimethyl-formamide; mineral oil T=80°C; 48 h; Show Experimental Procedure
参考文献
F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; LYNCH, Stephen M.; MARTIN, Rainer E.; NEIDHART, Werner; PLANCHER, Jean-Marc; SCHULZ-GASCH, Tanja Patent: WO2014/86663 A1, 2014 ; Location in patent: Page/Page column 71 ;
反应条件
Multi-step reaction with 6 steps 1: 60 percent / KF/Celite / acetonitrile / 1.) RT, 16 h, 2.) 70 deg C, 24 h2: 96 percent / CH2Cl2 / 68 h / Ambient temperature3: 95 percent / H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr4: 100 percent / methanol / 12 h / Ambient temperature5: 85 percent / CH2Cl2 / 1.5 h / Ambient temperature6: H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr
参考文献
Jasys, V. John; Kelbaugh, Paul B.; Nason, Deane M.; Phillips, Douglas; Rosnack, Kenneth J.; Saccomano, Nicholas A.; Stroh, Justin G.; Volkmann, Robert A. Journal of the American Chemical Society, 1990 , vol. 112, # 18 p. 6696 - 6704
反应条件
Multi-step reaction with 9 steps 1: 60 percent / KF/Celite / acetonitrile / 1.) RT, 16 h, 2.) 70 deg C, 24 h2: 96 percent / CH2Cl2 / 68 h / Ambient temperature3: 95 percent / H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr4: 100 percent / methanol / 12 h / Ambient temperature5: 85 percent / CH2Cl2 / 1.5 h / Ambient temperature6: H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr7: methanol / 12 h / Ambient temperature8: H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr9: 1.) N-hydroxysuccinimide, dicyclohexylcarbodiimide (DCC) / 1.) CH2Cl2, 3 h, 2.) RT, 12 h
参考文献
Jasys, V. John; Kelbaugh, Paul B.; Nason, Deane M.; Phillips, Douglas; Rosnack, Kenneth J.; Saccomano, Nicholas A.; Stroh, Justin G.; Volkmann, Robert A. Journal of the American Chemical Society, 1990 , vol. 112, # 18 p. 6696 - 6704
反应条件
Multi-step reaction with 8 steps 1: 60 percent / KF/Celite / acetonitrile / 1.) RT, 16 h, 2.) 70 deg C, 24 h2: 96 percent / CH2Cl2 / 68 h / Ambient temperature3: 95 percent / H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr4: 100 percent / methanol / 12 h / Ambient temperature5: 85 percent / CH2Cl2 / 1.5 h / Ambient temperature6: H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr7: methanol / 12 h / Ambient temperature8: H2 / Pd(OH)2/C / acetic acid / 2 h / 2585.7 Torr
参考文献
Jasys, V. John; Kelbaugh, Paul B.; Nason, Deane M.; Phillips, Douglas; Rosnack, Kenneth J.; Saccomano, Nicholas A.; Stroh, Justin G.; Volkmann, Robert A. Journal of the American Chemical Society, 1990 , vol. 112, # 18 p. 6696 - 6704