反应详情

To 2-cyanobenzene-1-sulfonyl chloride (201 mg, 1.00 mmol) in THF (5 mL), triethylamine (0.84 mL, 6.00 mmol) and 4-trifluoromethylpiperidine hydrochloride (284 mg, 1.50 mmol) were added. After stirring for 2 h, the reaction was concentrated and diluted with ethyl acetate and washed with water. After drying (Na2SO4), filtering, and concentrating, the residue was purified via silica gel chromatography eluting with 45% ethyl acetate/hexanes to provide 2-(4-(trifluoromethyl)piperidin-1-ylsulfonyl)benzonitrile [95 mg, LC-MS: 319.19 (M+H)+]. The product (52 mg) was dissolved in MeOH (5 mL), conc. HCl (25.0 mg) was added, and the whole was hydrogenated at 50 psi overnight. The reaction was concentrated and purified via preparative HPLC(CH3CN/water/TFA) to provide 210A. LC-MS: 323.21 (M+H)+.

1. concentrationthe reaction was concentrated
2. additiondiluted with ethyl acetate
3. washwashed with water
4. dry with materialAfter drying (Na2SO4)
5. filtrationfiltering
6. concentrationconcentrating
7. customthe residue was purified via silica gel chromatography
8. washeluting with 45% ethyl acetate/hexanes