反应详情

温度

40 °C

To a solution of methyl 3-aminothiophene-2-carboxylate (0.55 g; 3.5 mmol) in pyridine (2 mL) and dichloromethane (2 mL) was added 4-tert-butylbenzenesulfonyl chloride (0.98 g; 4.2 mmol). The resulting mixture was warmed to 40° C. to aid in solubility, then stirred at room temperature for 48 hours. The reaction mixture was diluted with dichloromethane and washed with aqueous hydrochloric acid (2N). The aqueous layer was separated and extracted with dichloromethane. The organic layers were combined, dried over anhydrous sodium sulfate, decanted, and filtered through a and of silica. The silica was washed with dichloromethane. The eluant was combined with hexanes and allowed to stand. After 24 hours the resulting solid product was collected by filtration to give the desired product as a white solid (817 mg).

1. washwashed with aqueous hydrochloric acid (2N)
2. customThe aqueous layer was separated
3. extractionextracted with dichloromethane
4. dry with materialdried over anhydrous sodium sulfate
5. customdecanted
6. filtrationfiltered through a and of silica
7. washThe silica was washed with dichloromethane
8. filtrationAfter 24 hours the resulting solid product was collected by filtration