反应详情

温度

100 °C

A mixture of 2.2 g of 1-(4-acetylaminophenyl)-3-allyl-3-azabicyclo[3.1.0]hexane-2,4-dione, 8 ml of water and 8 ml of concentrated hydrochloric acid is stirred for 3 hours at 100° C. The mixture is diluted with a small amount of water, cooled in an ice-water bath, made alkaline with 30% sodium hydroxide solution, and extracted twice with ethyl acetate. The organic phases are washed repeatedly with water and once with a concentrated aqueous solution of sodium chloride, dried over magnesium sulfate and filtered. The filtrate is concentrated and the residue is crystallised from ethyl acetate/petroleum ether. The title compound is obtained in the form of pale beige-coloured crystals with m.p. 104°-106° C. and with Rf=0.57 on thin-layer silica gel plates in the system methylene chloride/methanol (10:1).

1. temperaturecooled in an ice-water bath
2. extractionextracted twice with ethyl acetate
3. washThe organic phases are washed repeatedly with water and once with a concentrated aqueous solution of sodium chloride
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationThe filtrate is concentrated
7. customthe residue is crystallised from ethyl acetate/petroleum ether