反应详情

To a suspension of 0.44 g of 60% (w/w) sodium hydride in 49 ml of tetrahydrofuran is added 4.85 g of 5-chloro-3-(2-tritylamino-3-hydroxypropoxy)-1,2-benzoisoxazole at 20°-25° C. and they are refluxed for one hour. The reaction mixture is cooled to 5°-10° C., and thereafter, 1.56 g of methyl iodide is added, after which they are subjected to reaction at 20°-25° C. for five hours. The solvent is removed from the reaction mixture by distillation under reduced pressure, ethyl acetate and water are added to the residue obtained, 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. The residue obtained is crystallized from n-hexane and the crystals are collected by filtration, to obtain 5-chloro-3-(3-methoxy-2-tritylaminopropoxy)-1,2-benzoisoxazole.

1. temperaturethey are refluxed for one hour
2. temperatureThe reaction mixture is cooled to 5°-10° C.
3. customafter which they are subjected to reaction at 20°-25° C. for five hours
4. customThe solvent is removed from the reaction mixture by distillation under reduced pressure, ethyl acetate and water
5. additionare added to the residue
6. customobtained
7. customthe organic layer is separated
8. washThe separated organic layer is washed with a saturated saline solution
9. dry with materialdried over anhydrous magnesium sulfate
10. customafter which the solvent is removed by distillation under reduced pressure
11. customThe residue obtained
12. customis crystallized from n-hexane
13. filtrationthe crystals are collected by filtration