反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 100 ml of tetrahydrofuran, 20.1 g of vinylbenzylamine, 16.7 g of triethylamine, and 0.1 g of hydroquinone was placed in a reactor, and while cooling with ice water, a solution of 36.1 g of β-chloroethylsulfonylpropionic acid chloride 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 1,500 ml of ice water, and a precipitate was filtered off. The precipitate was recrystallized from a mixed solvent 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%. Elemental analysis (found): H, 5.74; C, 53.47; N, 4.83; Cl, 10.99; S, 10.49.
WORKUP
后处理
- customwas placed in a reactor
- waitto stand overnight at room temperature
- additionThe reaction mixture was then poured into a solution
- customprepared
- filtrationa precipitate was filtered off
- customThe precipitate was recrystallized from a mixed solvent of 200 ml of ethanol and 200 ml of water