HRID81343

反应详情

EQUATION

反应方程式

HRID 81343 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Ethyl-2-acetyl-6-nitrobenzoate (11.12 g) is suspended in a mixture of MeOH (70 mL) and MgSO4. Methylamine (2 molar in THF, 28.13 mL) is added dropwise and the solution is stirred for 15 min at this temperature. Then it is preheated to 70° C. for 18 h. The solvent is eliminated in vacuo, the residue is taken up in dichloromethane (100 mL), washed with sodium chloride solution (10%) dried on magnesium sulphate, filtered off from the desiccant and the solvent is eliminated in vacuo. For purification it is recrystallised from toluene (250 mL).

WORKUP

后处理

  1. waitThen it is preheated to 70° C. for 18 h
  2. washwashed with sodium chloride solution (10%)
  3. customdried on magnesium sulphate
  4. filtrationfiltered off from the desiccant and the solvent
  5. customFor purification it
  6. customis recrystallised from toluene (250 mL)