反应详情

温度

0 °C

A mixture of 3,4,5-trimethoxytoluene (1.86 g; 10.2 mmol), 1B (10.2 mmol), aluminium chloride (1.33 g, 10 mmol) and dichloromethane (20 ml) is stirred at 0° C. Subsequently, the reaction mixture is stirred for another 4 hours at room temperature. A mixture of dilute hydrochloric acid and ethyl acetate (1:1 v/v; 100 ml) is then slowly added at 0° C. The organic phase is concentrated and the residue is recrystallized from methanol. The solid material is collected by vacuum filtration, three times washed with methanol/water (3:1 v/v; 100 ml each) and dried yielding white crystals, 1.0 g (30.3%), mp 84° C.

1. stirringSubsequently, the reaction mixture is stirred for another 4 hours at room temperature
2. additionis then slowly added at 0° C
3. concentrationThe organic phase is concentrated
4. customthe residue is recrystallized from methanol
5. filtrationThe solid material is collected by vacuum filtration, three times
6. washwashed with methanol/water (3:1 v/v; 100 ml each)
7. customdried
8. customyielding white crystals, 1.0 g (30.3%), mp 84° C.