氯[3-(二甲基氨基)丙基]镁合成路线 （共 34 条）
反应条件
1: 3-(N,N-dimethylamino)-propylmagnesium chloride; C27H28BFN2O3 in tetrahydrofuran; water; toluene T=-40 - -35°C; 0.666667 - 0.833333 h; 2: With sulfuric acid in tetrahydrofuran; water; toluene pH=~ 2; 0.0833333 h; 3: 2,2,2-trimethylacetic acid With ammonia Product distribution / selectivity; more than 3 stages;
参考文献
SANDOZ AG
Patent: WO2007/82771 A1, 2007 ;
Location in patent: Page/Page column 24-25 ;
反应条件
1: 4-(4-fluorobenzoyl)-3-(hydroxymethyl)benzonitrile With (1S,2R)-(+)-N-methylephedrine in toluene T=20 - 70°C; 0.75 h; 2: 3-(N,N-dimethylamino)-propylmagnesium chloride in tetrahydrofuran; toluene T=-80°C; 0.2 h; Product distribution / selectivity;
参考文献
SANDOZ AG
Patent: WO2007/82771 A1, 2007 ;
Location in patent: Page/Page column 21 ;
反应条件
in tetrahydrofuran; toluene T=-60°C; 0.25 h; Product distribution / selectivity;
参考文献
SANDOZ AG
Patent: WO2007/82771 A1, 2007 ;
Location in patent: Page/Page column 20-21 ;
反应条件
1: 4-(4-fluorobenzoyl)-3-(hydroxymethyl)benzonitrile With (1S,2R)-(+)-N-methylephedrine in toluene T=20 - 70°C; 0.75 h; 2: 3-(N,N-dimethylamino)-propylmagnesium chloride in tetrahydrofuran; toluene T=-80°C; 0.2 h; Product distribution / selectivity;
参考文献
SANDOZ AG
Patent: WO2007/82771 A1, 2007 ;
Location in patent: Page/Page column 21 ;
反应条件
hydrogenchloride 1.) THF, toluene, 65 deg C, 2 h, 2.) 1 h, 3.) 75 deg C, 1.5 h, ethanol; Multistep reaction;
参考文献
Jalander, Lars; Oksanen, Lasse; Taehtinen, Johanna
Synthetic Communications, 1989 , vol. 19, # 19 p. 3349 - 3352
反应条件
1.1: tetrahydrofuran / 0.25 h / -5 °C 1.2: 0.5 h / -5 - 20 °C 1.3: pH 2 2.1: sulfuric acid / water / 6 h / 70 °C 3.1: hydrogen bromide / isopropyl alcohol; acetic acid / 1 h / 20 - 70 °C / pH ~ 2 View Scheme
参考文献
SHODHANA LABORATORIES LIMITED
Patent: US2011/92719 A1, 2011 ;
反应条件
ammonium chloride in tetrahydrofuran; water; toluene
参考文献
ORION CORPORATION FERMION
Patent: US2002/115872 A1, 2002 ;
反应条件
ammonium chloride in tetrahydrofuran
参考文献
H. Lundbeck A/S
Patent: US2002/35277 A1, 2002 ;
反应条件
1.1: tetrahydrofuran / 0.25 h / -5 °C 1.2: 0.5 h / -5 - 20 °C 1.3: pH 2 2.1: sulfuric acid / water / 6 h / 70 °C View Scheme
参考文献
SHODHANA LABORATORIES LIMITED
Patent: US2011/92719 A1, 2011 ;
反应条件
1.1: tetrahydrofuran / 0.25 h / -5 °C 1.2: 0.5 h / -5 - 20 °C 1.3: pH 2 2.1: isopropyl alcohol / 3 h / 20 - 45 °C 3.1: ammonia / water / pH ~ 9 3.2: 3 h / -5 °C View Scheme
参考文献
SHODHANA LABORATORIES LIMITED
Patent: US2011/92719 A1, 2011 ;
