反应详情

温度

-40 °C

10.0 g (0.026 Mol) 4-(2-Bromo-6-pyrrolidin-1-yl-pyridine-4-sulfonyl)-phenylamine were dissolved in tetrahydrofuran (200 ml), cooled at -40° C. and 33 ml (0.053 Mol) nBuLi in hexane were added. The reaction mixture was stirred at -15° C. for 1 h. Then water (10 ml) was added, the mixture was extracted with ethylacetate, the organic phase was washed with water and brine and dried over Na2SO4. After chromatography on SiO2 with ethyl acetate hexan 1:1 and drying in a high vacuum, it was obtained 3.6 g (45%) of 4-(2-pyrrolidin-1-yl-pyridine-4-sulfonyl) -phenylamine as light yellow cristals; mp.: 186-187° C.

1. extractionthe mixture was extracted with ethylacetate
2. washthe organic phase was washed with water and brine
3. dry with materialdried over Na2SO4
4. dry with materialAfter chromatography on SiO2 with ethyl acetate hexan 1:1 and drying in a high vacuum