反应详情

A mixture of the product from Example 50A (158 mg, 1 mmol) and Lawesson's reagent (808 mg, 2 mmol) in tetrahydrofuran (4 mL) was heated at reflux for 2 hours. The solution was concentrated, dissolved in dichloromethane (15 mL) and washed with saturated sodium bicarbonate solution (10 mL). The resulting organic layer was passed through a silica pad and washed with dichloromethane and ethyl acetate (10:1). The solvent was evaporated to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.39 (s, 9 H) 2.67 (s, 3 H); MS (ESI) m/z 157 (M+H)+.

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. concentrationThe solution was concentrated
4. dissolutiondissolved in dichloromethane (15 mL)
5. washwashed with saturated sodium bicarbonate solution (10 mL)
6. washwashed with dichloromethane and ethyl acetate (10:1)
7. customThe solvent was evaporated