反应详情

A solution of dimethylsulphamoyl chloride (0.107 ml) in dry dichloromethane was added to a stirred solution of 2,3,4,5-tetrahydro-5-methyl-2-[(5-methyl-1H-imidazol-4-yl)methyl]-1H-pyrido[4,3-b]indol-1-one (0.294 g) and triethylamine (0.2 ml) in dry dichloromethane (30 ml) under nitrogen, and the mixture was heated at reflux for ca. 24 h. After cooling the solution was concentrated onto FCC silica and purified by FCC eluting with System A (150:8:1) to give an oil. This oil was triturated with ether to give a solid which was further purified by slow evaporation from a solution in ethyl acetate to give the title compound (122 mg), m.p. 194°-196°, t.l.c. (System A, 100:8:1) Rf 0.43.

1. temperaturethe mixture was heated
2. temperatureat reflux for ca. 24 h
3. temperatureAfter cooling the solution
4. concentrationwas concentrated onto FCC silica
5. custompurified by FCC
6. washeluting with System A (150:8:1)
7. customto give an oil
8. customThis oil was triturated with ether
9. customto give a solid which
10. customwas further purified by slow evaporation from a solution in ethyl acetate