反应详情

温度

110 °C

4-Hydroxymethyl-3-(2,3,4-trifluorophenyl)-2(3H)-thiazolethione (60 g) prepared in the same manner as in Reference Example 19 was dissolved in N,N-dimethylformamide (450 ml) and thereto potassium carbonate (60 g) was added and the mixture was stirred at 110° C. for 3 hours. After the reaction mixture was evaporated to dryness, water was added to the residue and the resultant was extracted with chloroform. The extract was washed with a NaCl solution and dried over anhydrous sodium sulfate, followed by distilling off the solvent under reduced pressure. The residue was recrystallized from a mixed solvent of hexane-ethyl acetate to give the title compound (51 g) as pale yellow crystals, m.p. 163°-167° C.

1. customAfter the reaction mixture was evaporated to dryness, water
2. additionwas added to the residue
3. extractionthe resultant was extracted with chloroform
4. washThe extract was washed with a NaCl solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationby distilling off the solvent under reduced pressure
7. customThe residue was recrystallized from a mixed solvent of hexane-ethyl acetate