反应详情

Methyl 4-bromo-3-hydroxy-5-methyl-2-thiophenecarboxylate (2.5 g, 10 mmoles) is stirred under argon in DMF (20 mL). Dimethylthiocarbamyl chloride (2.65 g, 21 mmoles) and 1,4-diazabicyclo[2.2.2]octane (2.4 g, 21 mmoles) are added. The mixture is stirred at room temperature for 2 hours, then at 50° C. for 20 hours, then poured into ice water (200 mL) and extracted twice with toluene. The combined extracts are washed successively with 2N HCl, water, 0.5 M NaHCO3, and water, then dried over MgSO4. Removal of the solvent under reduced pressure, followed by recrystallization from ethyl acetate affords the product (2.7 g); mp 152°-154° C.

1. waitat 50° C. for 20 hours
2. extractionextracted twice with toluene
3. washThe combined extracts are washed successively with 2N HCl, water, 0.5 M NaHCO3, and water
4. dry with materialdried over MgSO4
5. customRemoval of the solvent under reduced pressure
6. customfollowed by recrystallization from ethyl acetate