HRID251925

反应详情

EQUATION

反应方程式

HRID 251925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.05 g of 6-chloro-8-methyl-1H-benzo[d]-1,3-oxazine-2,4-dione, 0.46 g of methyl carbazate and 20 ml of methanol was heated to reflux for 3 hours. After the reaction mixture was allowed to cool to around room temperature, water was poured thereto and the mixture was extracted with ethyl acetate three times. The resulting organic layer was concentrated under reduced pressure, and the residue was washed with toluene to obtain 0.77 g of N-(2-amino-5-chloro-3-methylbenzoyl)-N′-methoxycarbonylhydrazine of the formula:

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 3 hours
  3. temperatureto cool to around room temperature
  4. extractionthe mixture was extracted with ethyl acetate three times
  5. concentrationThe resulting organic layer was concentrated under reduced pressure
  6. washthe residue was washed with toluene