反应详情

Add thionyl chloride (3.1 mL, 0.0425 mol) dropwise to a stirred suspension of 8-chloro-5,11-dihydro[1]benzothiepino[4,3-b]pyridin-11-ol (8.8 g, 0.0334 mol) in CH2Cl2 (75 mL) at 3°-8° C. Stir the mixture at room temperature for 3 hours, and pour it into 150 mL of 2.5M NaOH containing ice. Filter, separate the aqueous layer and extract it with CH2Cl2 (2×50 mL). Combine the organic extracts, and wash with water (3×50 mL) and brine (1×75 mL). Dry the mixture over MgSO4, filter, and concentrate in vacuo to obtain the title compound (8.0 g, 80%).

1. additioncontaining ice
2. filtrationFilter
3. customseparate the aqueous layer
4. extractionextract it with CH2Cl2 (2×50 mL)
5. washCombine the organic extracts, and wash with water (3×50 mL) and brine (1×75 mL)
6. dry with materialDry the mixture over MgSO4
7. filtrationfilter
8. concentrationconcentrate in vacuo