反应详情

To a solution of 0.8 g of 5-chloro-3-(2-tert-butoxycarbonylamino-3-hydroxypropoxy)-1,2-benzoisoxazole in 8 ml of N,N-dimethylformamide are added 1.6 ml of triethylamine and 0.51 g of methyl isothiocyanate at room temperature, and they are subjected to reaction at 110° C. for four hours. After cooling, water and ethyl acetate are added to the reaction mixture, they are shaken and the organic layer is separated. The separated organic layer is washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure. The residue obtained is purified by a silica gel column chromatography [eluant:toluene:ethyl acetate=5:1], to obtain 0.4 g of brown, solid 5-chloro-3-(2-tert-butoxy carbonylamino-3-methylthiocarbamoyloxypropoxy)-1,2-benzoisoxazole.

1. customthey are subjected to reaction at 110° C. for four hours
2. temperatureAfter cooling
3. customthe organic layer is separated
4. washThe separated organic layer is washed with a saturated saline solution
5. dry with materialdried over anhydrous magnesium sulfate
6. customafter which the solvent is removed by distillation under reduced pressure
7. customThe residue obtained
8. customis purified by a silica gel column chromatography [eluant:toluene:ethyl acetate=5:1]