反应详情

In an argon atmosphere, 3-bromo-2-(4-chlorophenylthio)-5-dimethoxymethylthiophene (500 mg, 1.32 mmol) obtained in Example 90 was dissolved in tetrahydrofuran (6 mL) and cooled to −78° C. n-Butyl lithium (a 1.6 mol/L hexane solution, 0.81 mL, 1.3 mmol) and tetrahydrofuran (1 mL) solution of 4-chloro-N-methoxy-N-methylbenzamide (528 mg, 2.64 mmol) were added thereto, followed by stirring for 10 minutes. Water was added to the reaction liquid and the product was extracted with ethyl acetate. The organic layer was washed with water and brine, and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (15:1 hexane/ethyl acetate) to give 3-(4-chlorobenzoyl)-2-(4-chlorophenylthio)-5-dimethoxymethylthiophene (345 mg, 60%).

1. additionwere added
2. extractionthe product was extracted with ethyl acetate
3. washThe organic layer was washed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (15:1 hexane/ethyl acetate)