反应详情

A mixture of the product of Example 1, Step 6 (0.1 g, 0.29 mmol) and methane sulphonyl chloride (0.023 ml, 0.3 mmol) in dichloromethane (3 ml) was stirred at room temperature for 2 hours. The reaction was then poured into ethyl acetate, washed with water and aqueous sodium hydrogen carbonate solution, dried (MgSO4) and concentrated in vacuo. The crude residue was then purified by silica gel chromatography eluting with a 1:9:90 mixture of 0.88 ammonia solution:methanol:dichloromethane to give the title compound (0.075 g, 61%) as a yellow solid; MS(AP+) m/e 425 [M+H]+.

1. washwashed with water and aqueous sodium hydrogen carbonate solution
2. dry with materialdried (MgSO4)
3. concentrationconcentrated in vacuo
4. customThe crude residue was then purified by silica gel chromatography
5. washeluting with a 1:9:90 mixture of 0.88 ammonia solution