N,N-二甲氨基氯丙烷盐酸盐合成路线 (共 48 条)
反应条件
1.1: sodium iodide / acetonitrile / 132 h / Reflux 1.2: 0.5 h / 20 - 45 °C 2.1: lithium hexamethyldisilazane / toluene / 1 h / 20 °C 2.2: 2.5 h / 20 °C 3.1: tetrabutyl-ammonium chloride; potassium carbonate / water; acetonitrile / 0.25 h / 20 °C 3.2: 24 h / 60 °C 4.1: sodium hydroxide / methanol; water / 3 h / 20 °C 4.2: 0.08 h View Scheme
参考文献
Bosch, Joan; Bachs, Jordi; Gomez, Antonia M.; Griera, Rosa; Ecija, Marta; Amat, Mercedes
Journal of Organic Chemistry, 2012 , vol. 77, # 14 p. 6340 - 6344
反应条件
1.1: potassium hydroxide / water / 0 - 5 °C 1.2: 4 h / 100 - 110 °C / Reflux 2.1: tetrahydrofuran / 0.25 h / -5 °C 2.2: 0.5 h / -5 - 20 °C 2.3: pH 2 View Scheme
参考文献
SHODHANA LABORATORIES LIMITED
Patent: US2011/92719 A1, 2011 ;
反应条件
sodium hydroxide in benzene
参考文献
Boissier; Ratouis; Dumont; Taliani; Forest
Journal of medicinal chemistry, 1967 , vol. 10, # 1 p. 86 - 91
反应条件
1.1: potassium hydroxide / water / 0 - 5 °C 1.2: 4 h / 100 - 110 °C / Reflux 2.1: tetrahydrofuran / 0.25 h / -5 °C 2.2: 0.5 h / -5 - 20 °C 2.3: pH 2 3.1: isopropyl alcohol / 3 h / 20 - 45 °C 4.1: ammonia / water / pH ~ 9 4.2: 3 h / -5 °C 5.1: isopropyl alcohol / 0.5 h / 50 - 60 °C View Scheme
参考文献
SHODHANA LABORATORIES LIMITED
Patent: US2011/92719 A1, 2011 ;
反应条件
in tetrahydrofuran; water; N,N-dimethyl-formamide
参考文献
Kyowa Hakko Kogyo Co., Ltd.
Patent: US5698560 A1, 1997 ;
反应条件
sodium methylate in isopropyl alcohol T=100°C; 5 h;
参考文献
SENTINEL ONCOLOGY LIMITED
Patent: WO2007/144579 A1, 2007 ;
Location in patent: Page/Page column 49-50 ;
WO 2007/144579 A1
反应条件
1: 2-amino-phenol With sodium isopropanolate in isopropyl alcohol T=20°C; 2: 3-(dimethyl-amino)-propylchloride hydrochloride in isopropyl alcohol; toluene Reflux;
参考文献
Yang, Qingang; Chen, Lili; He, Xuchang; Gao, Zhenting; Shen, Xu; Bai, Donglu
Chemical and Pharmaceutical Bulletin, 2008 , vol. 56, # 10 p. 1400 - 1405
反应条件
1: 1.) EtONa / 1.) EtOH, 1 h, 2.) EtOH, reflux, 18 h
2: 1.) aq. KOH, 3.) aq. HCl
3: polyphosphoric ester / CHCl3 / 8 h / Heating
View Scheme
参考文献
Moloney, Gerard P.; Robertson, Alan D.; Martin, Graeme R.; MacLennan, Steven; Mathews, Neil; Dodsworth, Susan; Sang, Pang Yih; Knight, Cameron; Glen, Robert
Journal of Medicinal Chemistry, 1997 , vol. 40, # 15 p. 2347 - 2362
反应条件
sodium hydride
1.) DMF, 0 deg C, 10 min, 2.) 150 deg C, 2 h; Yield given. Multistep reaction;
参考文献
Couture; Grandclaudon
Synthesis, 1991 , # 11 p. 982 - 984
反应条件
potassium carbonate
Heating;
参考文献
Parimoo; Grabowski; Haney Jr.
Journal of pharmaceutical sciences, 1972 , vol. 61, # 6 p. 974 - 976