反应详情

A solution of 20 mg of 3-styryl-1H-indazol-5-ol, 5.76 mg of imidazole and 20.7 mg of methylphenylphosphinic chloride in 5 ml of dichloromethane is stirred at ambient temperature. After stirring for approximately one hour, 5.76 mg of imidazole and 20.7 mg of methylphenylphosphinic chloride are added. The suspension is stirred at ambient temperature for approximately 18 hours. 10 mg of imidazole and 70 mg of methylphenylphosphinic chloride are added. After 30 hours at ambient temperature, the reaction medium is treated with 10 ml of distilled water. The aqueous phase is extracted with 2×10 ml of dichloromethane. The organic phase is dried over magnesium sulfate and concentrated under reduced pressure in a rotary evaporator. The reaction crude is purified by preparative LC/MS to obtain 9.1 mg of methylphenylphosphinic acid 3-((E)-styryl)-1H-indazol-5-yl ester.

1. stirringThe suspension is stirred at ambient temperature for approximately 18 hours
2. waitAfter 30 hours at ambient temperature
3. extractionThe aqueous phase is extracted with 2×10 ml of dichloromethane
4. dry with materialThe organic phase is dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure in a rotary evaporator
6. customThe reaction crude
7. customis purified by preparative LC/MS