HRID2095998

反应详情

EQUATION

反应方程式

HRID 2095998 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 styrene (6.79 g, 65.3 mmol) and sodium bicarbonate (32.1 g, powder) in acetonitrile (100 mL), 3-chloro-N-hydroxy-2-oxopropanimidoyl chloride (i.e. the product of Example 7, Step B) (10 g, 64.1 mmol) was added in 10 portions over 20 minutes. The reaction mixture was then stirred for an additional 1 h and filtered. The filtered solid was rinsed with acetonitrile, and the combined filtrates were concentrated under reduced pressure to leave an oil, which was triturated first with hexanes and then with 1-chlorobutane to give 13.6 g of the title compound as a white solid.

WORKUP

后处理

  1. additionwas added in 10 portions over 20 minutes
  2. filtrationfiltered
  3. washThe filtered solid was rinsed with acetonitrile
  4. concentrationthe combined filtrates were concentrated under reduced pressure
  5. customto leave an oil, which
  6. customwas triturated first with hexanes