HRID1498921

反应详情

EQUATION

反应方程式

HRID 1498921 的结构方程式

PROCEDURE

实验过程

Tetrahydrofuran (30 ml) and methylhydrazine (138 mg) were added to 2-[(4-methoxy-3-methylbenzyl)methylamino]isoindole-1,3-dione (621 mg) prepared in the Step 15-1-3, and the mixture was stirred at a room temperature for one hour. Another methylhydrazine (138 mg) was added thereto, the resulting mixture was stirred for 12 hours. The solvent was distilled off under a reduced pressure. Dichloromethane was added to the residue, and the insoluble matter was removed by filtration. The filtrate was concentrated under a reduced pressure and then purified by silica gel column chromatography (dichloromethane:methanol=20:1) to give the title compound (115 mg, 31%).

WORKUP

后处理

  1. customprepared in the Step 15-1-3
  2. stirringthe resulting mixture was stirred for 12 hours
  3. distillationThe solvent was distilled off under a reduced pressure
  4. additionDichloromethane was added to the residue
  5. customthe insoluble matter was removed by filtration
  6. concentrationThe filtrate was concentrated under a reduced pressure
  7. custompurified by silica gel column chromatography (dichloromethane:methanol=20:1)