反应详情

A mixture of 100 ml of tetrahydrofuran, 20.1 g of vinylbezylamine, 16.7 g of triethylamine, and 0.1 g of hydroquinone was placed in a reactor, and while cooling with ice water, a solution containing 36.1 g of β-chloroethylsulfonylpropionic acid chloride dissolved in 200 ml of tetrahydrofuran was added dropwise thereto over a period of 30 minutes. The resulting mixture was allowed to stand overnight at room temperature. The reaction mixture was then poured into a solution prepared by diluting 16.5 g of concentrated hydrochloric acid with 1.5 liters of ice water, and the thus formed precipitate was collected by filtration. The precipitate was recrystallized from a solvent mixture of 200 ml of ethanol and 200 ml of water to provide 26.8 g of N-vinylbenzyl-β-chloroethylsulfonyl propionic acid amide. Yield was 57%. Melting point was 107°-108° C.

1. customwas placed in a reactor
2. additionwas added dropwise
3. waitto stand overnight at room temperature
4. additionThe reaction mixture was then poured into a solution
5. customprepared
6. filtrationthe thus formed precipitate was collected by filtration
7. customThe precipitate was recrystallized from a solvent mixture of 200 ml of ethanol and 200 ml of water