HRID1498921
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customprepared in the Step 15-1-3
- stirringthe resulting mixture was stirred for 12 hours
- distillationThe solvent was distilled off under a reduced pressure
- additionDichloromethane was added to the residue
- customthe insoluble matter was removed by filtration
- concentrationThe filtrate was concentrated under a reduced pressure
- custompurified by silica gel column chromatography (dichloromethane:methanol=20:1)