反应详情

A mixture of 6,6-dimethyl-5,7-dioxaspiro[2.5]octane-4,8-dione (0.500 g, 2.94 mmol) and 4-aminobenzonitrile (1.04 g, 8.82 mmol) in ethanol (3 mL) was irradiated in a microwave oven for 3 minutes at 100° C. The solution was concentrated under reduced pressure and the residue was dissolved in a solution of sodium hydroxide 6N, washed with dichloromethane, acidified with a solution of sodium hydrogen phosphate (1M) to pH=2, extracted with ethyl acetate dried and concentrated under reduced pressure to yield 0.240 g (36%) of a brown solid, which was used in the next step without further purification.

1. customwas irradiated in a microwave oven for 3 minutes at 100° C
2. concentrationThe solution was concentrated under reduced pressure
3. dissolutionthe residue was dissolved in a solution of sodium hydroxide 6N
4. washwashed with dichloromethane
5. extractionextracted with ethyl acetate
6. customdried
7. concentrationconcentrated under reduced pressure