反应详情

温度

0 °C

To a solution of trans-4-{[2-(2-Amino-phenyl)-ethylamino]-methyl}-cyclohexanecarboxylic acid methyl ester (2.99 g, 7.97 mmol) in CH3CN (100 mL) at 0° C. under argon was added portion wise triphosgene (1.53 g, 5.15 mmol) over 30 min. The reaction mixture was stirred at 0° C. for 30 min, warmed to room temperature and stirred additionally for 7 h. Then an excess of TEA was added and a precipitate was formed. Solvent was removed under reduced pressure and the crude product purified by flash chromatography on silica to afford the titled compound (4.3 g, yield 59%).

1. temperaturewarmed to room temperature
2. stirringstirred additionally for 7 h
3. additionThen an excess of TEA was added
4. customa precipitate was formed
5. customSolvent was removed under reduced pressure
6. customthe crude product purified by flash chromatography on silica