反应详情

35% sodium hydroxide solution (10 ml) was added to a cooled (0° C.) solution of (S)-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)indolin-2-yl)methanol (3.3 mmol, 1.0 eq) and tetra-n-butylammonium chloride (1.1 mmol, 0.33 eq) in toluene (20 ml). tert-Butylbromoacetate (1.5 eq) was added slowly to this mixture and the mixture was stirred for 2 h at room temperature. The organic phase was separated off and the aqueous phase extracted with ethyl acetate. The combined organic phases were washed with water and saturated sodium chloride solution, dried over Na2SO4 and concentrated to small volume under vacuum. The crude product was processed by column chromatography. Yield: 50%

1. customThe organic phase was separated off
2. extractionthe aqueous phase extracted with ethyl acetate
3. washThe combined organic phases were washed with water and saturated sodium chloride solution
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to small volume under vacuum