反应详情

温度

-40 °C

To a mixture of Compound (1) (674 mg.) and N-methylmorpholine (202 mg.) in dichloromethane (30 ml.), there was added isobutyl chloroformate (273 mg.) at -15°~-20° C. and the mixture was stirred for 30 minutes at the same temperature. The mixture was cooled to -40° C., and to this, there was added trimethyl silyl ester of Compound (2), which was prepared from Compound (2) (910 mg.) and bis (trimethylsilyl) acetamide (3 ml.) by stirring in a mixture of dichloromethane (20 ml.) and N,N-dimethylformamide (2 ml.). This mixture was stirred for 1 hour at -15°~-20° C., and after evaporation of the solvent, the residue was dissolved in ethylacetate (100 ml.), and then the solution was washed successively with 2%-HCl and water, dried over MgSO4 and evaporated. The residue was pulverized with isopyropyl ether to give Compound (3) (1.25 g.).

1. stirringThis mixture was stirred for 1 hour at -15°~-20° C.
2. customafter evaporation of the solvent
3. dissolutionthe residue was dissolved in ethylacetate (100 ml.)
4. washthe solution was washed successively with 2%-HCl and water
5. dry with materialdried over MgSO4
6. customevaporated