反应详情

A solution of the product from Example 2, Step B (0.55 g, 1.45 mmol) in dichloromethane (20 mL) was cooled (ice bath), thionyl chloride (0.16 mL, 2.18 mmol) was added, and the mixture was stirred for thirty minutes. The reaction mixture was evaporated to a residue which was dissolved in dichloromethane (20 mL) and evaporated. A solution of sodium cyanide (0.29 g, 5.8 mmol) in DMSO (10 mL) was added to this residue and the mixture was stirred at room temperature for one hour. Saturated aqueous sodium bicarbonate (100 mL) was added and the mixture was extracted with ethyl acetate (3×100 mL). The combined extracts were washed with saturated aqueous sodium bicarbonate (2×150 mL), dried (MgSO4) and evaporated to a tan solid (0.49 g, 87%): LC/MS m/z 389 [M+H]+.

1. additionwas added
2. customThe reaction mixture was evaporated to a residue which
3. dissolutionwas dissolved in dichloromethane (20 mL)
4. customevaporated
5. stirringthe mixture was stirred at room temperature for one hour
6. extractionthe mixture was extracted with ethyl acetate (3×100 mL)
7. washThe combined extracts were washed with saturated aqueous sodium bicarbonate (2×150 mL)
8. dry with materialdried (MgSO4)
9. customevaporated to a tan solid (0.49 g, 87%)