HRID1577904

反应详情

EQUATION

反应方程式

HRID 1577904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 15.00 g (0.08 mole) of N-methyl-4-hydroxybenzenesulfonamide, 8.11 g (0.08 mole) of triethylamine and 200 ml of methylene chloride cooled to 0° C. was added a solution of 8.37 g (0.08 mole) of methacryloyl chloride in 100 ml of methylene chloride over a period of approximately 30 minutes. The solution was then stirred for another 3 hours with cooling; washed once with 100 ml of 2 percent HCl solution, and twice with water; dried over magnesium sulfate and concentrated in vacuo in a warm water bath. The resultant solid was recrystallized from 150 ml of ethyl alcohol:water (1:1) with filtering through diatomaceous earth. Collection of the white solid and drying at room temperature in vacuo gave 16.20 g (79.9 percent of theory) of N-methyl-4-methacryloyloxybenzenesulfonamide; m.p.=106° to 107° C.

WORKUP

后处理

  1. temperaturewith cooling
  2. washwashed once with 100 ml of 2 percent HCl solution
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo in a warm water bath
  5. customThe resultant solid was recrystallized from 150 ml of ethyl alcohol:water (1:1)
  6. filtrationwith filtering through diatomaceous earth
  7. customCollection of the white solid
  8. customdrying at room temperature in vacuo