反应详情

A solution of the compound obtained in Example 1, Step e (75.9 mg) in methylene chloride (2 ml) was added with triphosgene (89 mg, Tokyo Kasei Kogyo) and triethylamine (140 μl) and stirred for 2 hours under ice cooling. The reaction mixture was added with 2,2,2-trifluoroethanol (47 μl, Tokyo Kasei Kogyo) and stirred for three days. The reaction mixture was diluted with methylene chloride, washed with 1 N HCl and saturated aqueous sodium hydrogencarbonate in this order, dried over magnesium sulfate and concentrated. The obtained residue was applied to a silica gel column and eluted with hexane/ethyl acetate (5:1) to obtain the title compound (48.5 mg).

1. stirringstirred for three days
2. washwashed with 1 N HCl and saturated aqueous sodium hydrogencarbonate in this order
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated
5. washeluted with hexane/ethyl acetate (5:1)