反应详情

A mixture of 4-bromo-2,2,6,6-tetramethyl-3,5-heptanedione(α-bromo-dipivaloylmethane; 1.42 g, 5.40 mmol), thiourea (451.8 mg, 5.94 mmol) and ethanol (15 mL) was refluxed for 2 hours. After cooling, the reaction mixture was poured into saturated aqueous sodium hydrogen carbonate and extracted with ethyl acetate. After the organic layer was washed with water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation under reduced pressure was crystallized (dichloromethane/hexane) to give the title compound (1.23 g, 94.5%) as a white crystal.

1. temperaturewas refluxed for 2 hours
2. temperatureAfter cooling
3. extractionextracted with ethyl acetate
4. washAfter the organic layer was washed with water and brine
5. dry with materialdried over anhydrous sodium sulfate
6. customthe residue obtained by evaporation under reduced pressure
7. customwas crystallized (dichloromethane/hexane)