反应详情

To a stirred solution of 3-(2-bromo-5-chloro-4-(4-ethoxybenzyl)phenyl)propan-1-ol (BL) (0.268 g, 0.70 mmol) in 5 mL of THF was added NaH (0.034 g, 0.84 mmol, 60%) and stirred for 40 min. 1-bromo-2-butyne (0.094 mL, 1.05 mmol) was added and the mixture was stirred overnight at room temperature. The reaction was quenched with water and extracted with ethyl acetate. The combined organic layers were washed with water and brine, dried over Na2SO4, concentrated and purified by preparative TLC (eluting with EtOAc:PE=1:10) to obtain 0.2 g of intermediate BM.

1. stirringthe mixture was stirred overnight at room temperature
2. customThe reaction was quenched with water
3. extractionextracted with ethyl acetate
4. washThe combined organic layers were washed with water and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. custompurified by preparative TLC (eluting with EtOAc:PE=1:10)