Thionyl Chloride → (3-Chloro-propylamino)-(4-fluoro-phenyl)-acetic acid methyl ester
反応式
S(Cl)([Cl:3])=O.[CH3:5][O:6][C:7](=[O:21])[CH:8]([C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1)[NH:9][CH2:10][CH2:11][CH2:12]O>C(Cl)(Cl)Cl>[CH3:5][O:6][C:7](=[O:21])[CH:8]([NH:9][CH2:10][CH2:11][CH2:12][Cl:3])[C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1参加物
4
反応条件
- 温度
- 50 °C
実験手順
To a solution of thionyl chloride (8.79 g) in chloroform (20 mL) was added (4-fluoro-phenyl)-(3-hydroxy-propylamino)-acetic acid methyl ester (14.85 g, dissolved in 60 mL of chloroform) dropwise via syringe. The reaction mixture was then stirred for 1.5 hours at 50° C. and the volatiles were subsequently removed in vacuo to give a solid residue which was triturated with diethyl ether (30 mL) to give the desired HCl salt of (3-chloro-propylamino)-(4-fluoro-phenyl)-acetic acid methyl ester (14.88 g, MS (ES+): 260.1 (MH+)) as an off-white solid.