反应详情

To 250 mg of 3-(2,5-dimethyl-phenyl)-4-hydroxy-8-methoxy-1,8-diaza-spiro[4.5]dec-3-en-2-one in 2.5 ml of tetrahydrofuran are added 160 □l of Hünig's base and 85 □l of chloromethyl ethyl ether. After stirring for 20 hours at room temperature, water and ethyl acetate are added and the layers are separated. The aqueous phase is extracted with ethyl acetate, the combined organic phases dried with sodium sulfate, filtered and concentrated. Chromatography (heptane/acetone 4:1) yielded 72 mg of 3-(2,5-dimethyl-phenyl)-4-ethoxymethoxy-8-methoxy-1,8-diaza-spiro[4.5]dec-3-en-2-one as a solid, mp:150-152° C.

1. customthe layers are separated
2. extractionThe aqueous phase is extracted with ethyl acetate
3. dry with materialthe combined organic phases dried with sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated