反应详情

A solution of 4 g. (0.011 mole) of 3'-(2,4-dichlorophenyl)-spiro[isobenzofuran-1(3H),5'(4'H)-isoxazol]-3-one, 2 ml. of concentrated H2SO4 and 200 ml. of ethanol was held at reflux for 19 hours, cooled, and poured into ice water. The resultant mixture was extracted twice with ether. The ethereal solution was washed twice with water, dried over CaSO4 and concentrated under vacuum to give an oil. The oil was dissolved in hot hexane to afford 4.2 g. of a crystalline solid (96.9%). Recrystallization of the solid from hexane gave 3.1 g. of pure product; m.p. 85°-86° C.

1. temperatureat reflux for 19 hours
2. temperaturecooled
3. extractionThe resultant mixture was extracted twice with ether
4. washThe ethereal solution was washed twice with water
5. dry with materialdried over CaSO4
6. concentrationconcentrated under vacuum
7. customto give an oil
8. customto afford 4.2 g
9. customRecrystallization of the solid from hexane
10. customgave 3.1 g