反应详情

To a stirred 0° C. solution of Et3SiH (2.26 ml, 14.2 mmol) and (5-chloro-2-hydroxyphenyl)(4-ethylphenyl)methanone (1.944 g, 7.08 mmol) in 10 mL of TFA was added CF3SO3H (30 μL) at a rate to keep the temperature at about 0° C. After complete addition, the mixture was warmed to room temperature and stirred overnight at room temperature. After the volatiles were evaporated under reduced pressure, the residue was partitioned in ethyl acetate and water. The organic layer was separated and washed with water, aq Na2CO3, brine then dried over Na2SO4 and concentrated. The crude product was purified by column chromatography (PE:EA=10:1) to give the target compound (1.659 g).

1. customat about 0° C
2. additionAfter complete addition
3. customAfter the volatiles were evaporated under reduced pressure
4. customthe residue was partitioned in ethyl acetate
5. customThe organic layer was separated
6. washwashed with water, aq Na2CO3, brine
7. dry with materialthen dried over Na2SO4
8. concentrationconcentrated
9. customThe crude product was purified by column chromatography (PE:EA=10:1)