反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
N,N-dimethylformamide (20 ml), methyl iodide (0.7 ml) and potassium carbonate (3.12 g) were added to 2-(4-methoxy-3-methylbenzylamino)isoindole-1,3-dione (1.67 g) prepared in the Step 15-1-2, and the mixture was stirred overnight. Methyl iodide (0.35 ml) was added thereto, and the resulting mixture was stirred for another 5 hours. Thereafter, an ethyl acetate-toluene (3:1) solution was added thereto. The resulting mixture was washed with water and a saturated saline solution in order, and then dried over sodium sulfate and concentrated under a reduced pressure. To the resulting residue, diethyl ether was added, and the mixture was stirred at a room temperature. The precipitate was separated by filtration, washed with diethyl ether, and dried under a reduced pressure to give the title compound (1.15 g, 65%).
WORKUP
后处理
- customprepared in the Step 15-1-2
- stirringthe resulting mixture was stirred for another 5 hours
- washThe resulting mixture was washed with water
- dry with materiala saturated saline solution in order, and then dried over sodium sulfate
- concentrationconcentrated under a reduced pressure
- additionTo the resulting residue, diethyl ether was added
- stirringthe mixture was stirred at a room temperature
- customThe precipitate was separated by filtration
- washwashed with diethyl ether
- customdried under a reduced pressure