反应详情

A mixture of {5-[2-(6-cyano-thieno[3,2-b]pyridin-7-ylamino)-ethyl]-thiazol-2-yl}-carbamic acid tert-butyl ester (36.1 mg, 0.09 mmol) and trifluoroacetic acid (1 ml) in 4 ml of dichloromethane was stirred at room temperature for 16 hr. Dichloromethane was evaporated, and the residue obtained was dissolved in ethyl acetate, washed with aqueous sodium bicarbonate solution, dried over MgSO4, filtered, and concentrated in vacuum to give a yellow crude product 24 mg. (89%). 1H NMR (300 MHz, CD3OD) δ 8.85 (s, 1H), 8.46 (d, J=5.4 Hz, 1H), 7.59 (d, J=5.7 Hz, 1H), 7.14 (s, 1H), 4.19 (t, J=7.2 Hz, 2H), 3.22 (t, J=7.2 Hz, 2H); LC-MS (ESI) m/z 302.0 (M+1).

1. customDichloromethane was evaporated
2. customthe residue obtained
3. washwashed with aqueous sodium bicarbonate solution
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuum