反应详情

(5-Amino-2-trifluoromethoxyphenyl)methanol (1.2 g, 5.8 mmol) was dissolved in DMF (5 mL) and imidazole (0.48 g, 7.1 mmol) and tert-butyldimethylsilylchloride (0.99 g, 6.6 mmol) were added and the mixture was stirred for 16 hours. The reaction mixture was extracted with ethylacetate (50 mL) and water (20 mL). The aqueous phase was extracted once more with ethyl acetate (20 mL). The combined organic phases were washed with water (10 mL), aqueous citric acid (10 mL, 10%) and water (2×10 mL), dried (magnesium sulphate) and concentrated in vacuo. The residue was purified by column chromatography (110 g, silica gel) using ethyl acetate and heptane (1:3) as eluent to give 1.2 g of 3-(tert-butyldimethylsilanyloxymethyl)-4-trifluoromethoxyphenylaniline.

1. extractionThe reaction mixture was extracted with ethylacetate (50 mL) and water (20 mL)
2. extractionThe aqueous phase was extracted once more with ethyl acetate (20 mL)
3. washThe combined organic phases were washed with water (10 mL), aqueous citric acid (10 mL, 10%) and water (2×10 mL)
4. dry with materialdried (magnesium sulphate)
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography (110 g, silica gel)