HRID1282402

反应详情

EQUATION

反应方程式

HRID 1282402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

At 2° C., a solution of 79.5 g of sodium nitrite in 150 ml of water is added to a mixture of 185.5 g of methyl 2-amino-4-chlorobenzoate, 785 ml of water and 190.5 ml of concentrated sulfuric acid. Subsequently, the mixture is stirred for 30 minutes, and 5.3 g of amidosulfonic acid are then added. The resulting reaction mixture is added dropwise to 108.2 g of methyl acrylate. 766 mg of palladium acetylacetonate are then added to the reaction mixture, which is then heated to 40° C. After a further 3.5 hours at 40° C., the resulting precipitate is filtered off, giving, after drying, 248.3 g of methyl 4-chloro-2-(3-methoxy-3-oxo-1-propenyl)-benzoate of melting point 87-89° C.

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. waitAfter a further 3.5 hours at 40° C.
  3. filtrationthe resulting precipitate is filtered off
  4. customgiving
  5. customafter drying