反应详情

A solution of 1.00 g of 3-(2-tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole and 0.73 g of triethylamine in 5 ml of methylene chloride is added to a solution of 0.42 g of trichloromethyl chloroformate in 5 ml of methylene chloride at 5°-7° C. over 20 minutes, and they are subjected to reaction at the same temperature for 30 minutes. This solution is added to a solution of 1.20 g of methoxyamine hydrochloride and 0.78 g of sodium methoxide in 15 ml of methanol at -30° C. and the temperature is elevated to 0° C., at which they are subjected to reaction for 30 minutes. Water is added to the reaction mixture, and after shaking, 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 to obtain 3-(2-tert-butoxycarbonylamino-3-methoxyaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole.

1. customthey are subjected to reaction at the same temperature for 30 minutes
2. customis elevated to 0° C., at which they
3. customare subjected to reaction for 30 minutes
4. customthe organic layer is separated
5. washThe separated organic layer is washed with a saturated saline solution
6. dry with materialdried over anhydrous magnesium sulfate
7. customafter which the solvent is removed by distillation under reduced pressure