反应详情

A mixture of Example 39H (23.8 mg, 0.050 mmol), pyridine (31.6 mg, 0.80 mmol), and 1-naphthalenesulfonyl chloride (45.3 mg, 0.20 mmol) in acetone (1.5 mL) was stirred at rt for 72 h. The reaction mixture was evaporated in vacuo and partitioned between ethyl acetate and 1 N HCl. The organic phase was separated, dried (MgSO4), filtered, and evaporated in vacuo. The residue was purified by chromatography on silica gel eluting with 99:1 dichloromethane/methanol to provide the title compound (32.0 mg, quant. yield).

1. customThe reaction mixture was evaporated in vacuo
2. custompartitioned between ethyl acetate and 1 N HCl
3. customThe organic phase was separated
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated in vacuo
7. customThe residue was purified by chromatography on silica gel eluting with 99:1 dichloromethane/methanol