HRID441268

反应详情

EQUATION

反应方程式

HRID 441268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 33 g of m-nitro-acetylacetanilide, 38.1 g of methyl orthoformate and 13 drops of 36° Be sulfuric acid was allowed to stand for 16 hours and after the addition of 40 drops of quinoline and 150 ml of toluene, the mixture was heated to 130° C. while distilling of the methanol formed as an azeotrope. The mixture was cooled and vacuum filtered and the recovered precipitate was crystallized from acetone to obtain 24 g of m-nitro-3-methoxy-crotonanilide melting at 187° C.

WORKUP

后处理

  1. distillationwhile distilling of the methanol
  2. customformed as an azeotrope
  3. temperatureThe mixture was cooled
  4. filtrationvacuum filtered
  5. customthe recovered precipitate was crystallized from acetone