反应详情

2-Bromo-4,5-dimethoxylbenzeneethanamine (3.5 g 13.2 mmol) was dissolved and stirred in 50 mL dry acetonitrile. 2.14 mL (1.1 equiv) phthaloyl dichloride and 7 mL (3 equiv) Hünig's base were added. The mixture was stirred at room temperature overnight. Acetonitrile was removed; the remaining product was taken up in dichloromethane and washed with basic water (pH=11). The aqueous wash was extracted with dichloromethane 15 mL×3. The organic fractions were combined and dried over sodium sulfate. Solvent was removed to give the crude product, which was then purified by column chromatography. Calculated yield: 1.8 g (34%).

1. customAcetonitrile was removed
2. washwashed with basic water (pH=11)
3. washThe aqueous wash
4. extractionwas extracted with dichloromethane 15 mL×3
5. dry with materialdried over sodium sulfate
6. customSolvent was removed