反应详情

温度

80 °C

To a DMF (2 ml) solution of this amide (105 mg, 0.3 mmol) and 2-mercaptobenzoxazole (50 mg, 0.33 mmol) were added 18-crown-6 (8 mg, 0.03 mmol) and potassium carbonate (50 mg, 0.36 mmol), and the mixture was stirred at 80° C. for 3 hours. The reaction mixture was diluted with water, and then extracted with ethyl acetate. The organic layer was washed with water and then with a saturated aqueous solution of sodium chloride, and dried over sodium sulfate. Subsequently, the solvent was distilled off, and the resulting crude product was purified through preparative thin-layer chromatography (eluent—hexane:ethyl acetate=3:2, eluted twice) to obtain 67 mg (yield 53%) of the desired compound as a colorless needle crystal.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water
3. dry with materialwith a saturated aqueous solution of sodium chloride, and dried over sodium sulfate
4. distillationSubsequently, the solvent was distilled off
5. customthe resulting crude product was purified through preparative thin-layer chromatography (eluent—hexane
6. washethyl acetate=3:2, eluted twice)