反应详情

A mixture of triphenylphosphine oxide (2.1 g), trifluoromethanesulfonic anhydride (0.63 mL) and dichloromethane (35 mL) was stirred for 30 min under ice-cooling. 4-Methyl-7-[(2-thienylsulfonyl)amino]-N-[2-(tritylthio)ethyl]-1H-indole-2-carboxamide (0.80 g) was added, and the mixture was stirred for 90 min under ice-cooling. The reaction mixture was poured into aqueous sodium hydrogencarbonate solution and extracted with dichloromethane. The aqueous layer was extracted with dichloromethane, and the combined dichloromethane layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was subjected to silica gel column chromatography (ethyl acetate:hexane=3:7-5:5), and the obtained crystals were recrystallized from ethyl acetate-hexane to give the title compound (431 mg, yield 91%) as colorless prism crystals. melting point 198-199° C.

1. temperaturecooling
2. stirringthe mixture was stirred for 90 min under ice-
3. temperaturecooling
4. extractionextracted with dichloromethane
5. extractionThe aqueous layer was extracted with dichloromethane
6. dry with materialthe combined dichloromethane layer was dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customthe obtained crystals were recrystallized from ethyl acetate-hexane