反应详情

To a solution of methyl 4-bromo-1H-indole-2-carboxylate (4.09 g) in dichloromethane (60 mL) was added a mixture of POCl3 (3.7 g) and N,N-dimethylformamide (1.76 g). The mixture was stirred at reflux overnight. The mixture was diluted with ethyl acetate (300 mL) and 2M sodium acetate solution in water (200 mL). The mixture was stirred thoroughly for 1 hour. The aqueous layer was extracted with ethyl acetate. The combined extracts were washed with water (×3), brine and dried over Na2SO4. After filtration, concentration of the mixture gave the title compound, which was used in next step without purification.

1. temperatureat reflux overnight
2. stirringThe mixture was stirred thoroughly for 1 hour
3. extractionThe aqueous layer was extracted with ethyl acetate
4. washThe combined extracts were washed with water (×3), brine
5. dry with materialdried over Na2SO4
6. filtrationAfter filtration, concentration of the mixture