反应详情

Phosphoryl chloride (1.05 ml) was added dropwise to ice-cooled dimethylacetamide (10 ml) and the solution was stirred, in ice, for 5 min. A solution of 5-methoxy-1-methyl-1H-indole (1.4 g) in dimethylacetamide (5 ml) was added dropwise, and the resulting solution was stirred at 85° for 2 h, then cooled, and partitioned between sodium carbonate (2N; 100 ml) and ethyl acetate (2×100 ml). The combined organic extracts were washed with water (2×100 ml), dried and evaporated in vacuo. The residue was purified by FCC eluting with ethyl acetate to give a solid which was crystallised from a mixture of ethyl acetate and hexane to give the title compound (0.6 g), m.p. 167°-168°.

1. stirringthe resulting solution was stirred at 85° for 2 h
2. temperaturecooled
3. custompartitioned between sodium carbonate (2N; 100 ml) and ethyl acetate (2×100 ml)
4. washThe combined organic extracts were washed with water (2×100 ml)
5. customdried
6. customevaporated in vacuo
7. customThe residue was purified by FCC
8. washeluting with ethyl acetate
9. customto give a solid which
10. customwas crystallised from a mixture of ethyl acetate and hexane