反应详情

A solution of ethyl isonipecotate (27.6 g, 175 mmol) in dichloromethane (50 ml) was added dropwise over 10 minutes to a solution of 3-chlorobenzoyl chloride (20 ml, 160 mmol) and triethylamine (28 ml, 200 mmol) in dichloromethane (500 ml) cooled to between 10 and 15° C. The reaction was then stirred at room temperature for 3 hours and concentrated under reduced pressure. The residue was diluted with ether, the solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine. It was then dried over MgSO4 and evaporated under reduced pressure, to give the title compound as a solid, 44.49.

1. temperaturecooled to between 10 and 15° C
2. concentrationconcentrated under reduced pressure
3. additionThe residue was diluted with ether
4. washthe solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine
5. dry with materialIt was then dried over MgSO4
6. customevaporated under reduced pressure