HRID3078

反应详情

EQUATION

反应方程式

HRID 3078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 54.4 g of p-isobutyloxycarbonylaminophenyl sulfonamide, 40 g of triethylamine, 2 g of N,N-dimethylaminopyridine and 150 ml of N,N-dimethylacetamide was then added dropwise 22.8 g of methacrylic chloride under cooling with ice. After the completion of the dropwise addition, the reaction mixture was stirred for 2 hours. The reaction product was then poured into water. The resulting crystal was then withdrawn by filtration. The crystal was then recrystallized from a 3/7 (by volume) mixture of toluene and ethyl acetate to obtain 40 g of N-(p-isobutyloxycarbonylaminophenylsulfonyl)methacrylamide in the form of white crystal (m.p. 194°-196° C.).

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. additionAfter the completion of the dropwise addition
  3. customThe resulting crystal was then withdrawn by filtration
  4. customThe crystal was then recrystallized from a 3/7 (by volume) mixture of toluene and ethyl acetate