反应详情

温度

120 °C

A mixture of 2,5-difluoro-phenylamine (129 mg, 1 mmol) and potassium o-ethyl dithiocarbonate (352 mg, 2.2 mmol) in DMF (5 mL) was heated to 120° C. for 15 min in microwave. The reaction mixture was cooled, diluted with 10 mL of ice water, and acidified with 3 mL of HCl solution (1 mol/L). Then the mixture was extracted with EtOAc (3×50 mL), washed with brine and dried over Na2SO4. The dried organic layers were concentrated to give 5-fluorobenzo[d]thiazole-2-thiol (120 mg, 0.67 mmol, 67%). ESI-MS (M+1): 185 calc. for C7H4FN4S2 184.

1. temperatureThe reaction mixture was cooled
2. extractionThen the mixture was extracted with EtOAc (3×50 mL)
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. concentrationThe dried organic layers were concentrated