反应详情

2-[4-(4-Chloro-1,2-diphenyl-but-1-enyl)-phenoxy]-ethanol (Compound II) (0.3 g, 0.79 mmol) was dissolved in tetrahydrofuran (5 ml) under a nitrogen atmosphere. Sodium hydride (0.058 g, 1.21 mmol) was added in THF (5 ml) to the solution and the mixture was stirred at room temperature for an hour. Then the mixture was cooled to 0° C., ethyl bromo acetate (0.4 g, 2.38 mmol) was added and the stirring was continued for 5 hours at 0-5° C. The mixture was allowed to warm up to room temperature and stirring was continued overnight. Then the reaction is quenched with water and ethyl acetate. The aqueous layer was separated and extracted with ethyl acetate. The organic phase was washed with water, dried with sodium sulphate and evaporated to dryness. The residue was used in the next reaction step without further purification.

1. temperatureThen the mixture was cooled to 0° C.
2. temperatureto warm up to room temperature
3. stirringstirring
4. waitwas continued overnight
5. customThen the reaction is quenched with water and ethyl acetate
6. customThe aqueous layer was separated
7. extractionextracted with ethyl acetate
8. washThe organic phase was washed with water
9. dry with materialdried with sodium sulphate
10. customevaporated to dryness
11. customThe residue was used in the next reaction step without further purification