反应详情

温度

95 °C

To a solution of 2.0 g of 2-trichloroacetamido-3-benzoylthiophene in 18 ml of dimethylsulfoxide was added 0.89 g of ammonium acetate. The mixture was heated at 95° C for 2 hours, and poured into ice water, and extracted with chloroform. The chloroform layer was washed with water, dried over sodium sulfate, and the solvent was removed under reduced pressure. The residue was chromatographed on 60 g of silica gel, using methanol as an eluent to obtain 4-phenyl-1,2-dihydrothieno(2,3-d)-pyrimidin-2-one as crystals. Recrystallized from chloroform-acetone, the crystals having a melting point of 247.5°- 249° C. were obtained.

1. extractionextracted with chloroform
2. washThe chloroform layer was washed with water
3. dry with materialdried over sodium sulfate
4. customthe solvent was removed under reduced pressure
5. customThe residue was chromatographed on 60 g of silica gel