反应详情

To a solution of 0.24 g of 60% sodium hydride in 10 ml of N,N-dimethylformamide are dropwise added 2.0 g of 2-(2-methyl-1,3-thiazol-5-yl)-2-tritylaminoethanol, a solution of 10 ml of N,N-dimethylformamide at room temperature, and the temperature is gradually elevated to 80° C. after which 1.03 g of 3,5-dichloro-1,2-benzoisoxazole is added. They are subjected to reaction at the same temperature for one hour. After cooling, water and ethyl acetate are added, and the crystals precipitated are collected by filtration. The organic layer of the filtrate is separated, washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure. The crystals obtained are combined with the crystals previously collected by filtration to obtain 1.81 g of colorless, crystalline 5-chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-tritylaminoethoxy]-1,2-benzoisoxazole.

1. customat room temperature
2. customis gradually elevated to 80° C.
3. additionis added
4. customThey are subjected to reaction at the same temperature for one hour
5. temperatureAfter cooling
6. customthe crystals precipitated
7. filtrationare collected by filtration
8. customThe organic layer of the filtrate is separated
9. washwashed with a saturated saline solution
10. dry with materialdried over anhydrous magnesium sulfate
11. customafter which the solvent is removed by distillation under reduced pressure
12. customThe crystals obtained
13. filtrationpreviously collected by filtration