反应详情

温度

70 °C

Into a 100 ml flask, the product from step (c) (5.78 g, 14.93 mmol) dissolved in thionyl chloride (50 ml) was added. Pyridine (120 μL, 1.49 mmol) was added and the reaction mixture heated to 70° C. for 1 hour. The reaction mixture was allowed to cool to room temperature and the volatiles were evaporated in vacuo. The residue was partitioned between saturated aqueous Na2CO3 and EtOAc. The aqueous layer was extracted with EtOAc (3×). The combined EtOAc extracts were washed with brine, dried over Na2SO4, and solvent evaporated in vacuo to give the sub-title compound as an orange semi-solid (5.9 g) that was used directly in the next step. MS: ESI (positive): 405 (M+1).

1. additionwas added
2. temperatureto cool to room temperature
3. customthe volatiles were evaporated in vacuo
4. customThe residue was partitioned between saturated aqueous Na2CO3 and EtOAc
5. extractionThe aqueous layer was extracted with EtOAc (3×)
6. washThe combined EtOAc extracts were washed with brine
7. dry with materialdried over Na2SO4, and solvent
8. customevaporated in vacuo