反应详情

N-(2,4-dimethoxybenzyl)-5-(1-(tetrahydro-2H-pyran-4-yl)pyrrolidin-2-yl)-N-(thiazol-2-yl)naphthalene-2-sulfonamide (0.038 g, 0.065 mmol) was dissolved in DCM (1 mL) and TFA (0.1 ml, 1.298 mmol) was added. The reaction was stirred for 30 minutes at room temperature. The reaction was concentrated, triturated with diethyl ether, and filtered. The solids were washed with diethyl ether and vacuum dried overnight to afford 5-(1-(tetrahydro-2H-pyran-4-yl)pyrrolidin-2-yl)-N-(thiazol-2-yl)naphthalene-2-sulfonamide 2,2,2-trifluoroacetate as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm=12.79 (br. s., 1H), 9.65 (br. s., 1H), 8.55 (br. s., 1H), 8.43 (d, J=9.1 Hz, 1H), 8.27 (d, J=7.2 Hz, 1H), 8.04 (d, J=7.3 Hz, 1H), 7.91 (d, J=8.9 Hz, 1H), 7.82-7.72 (m, 1H), 7.27 (d, J=4.6 Hz, 1H), 6.85 (d, J=4.5 Hz, 1H), 5.61 (d, J=6.1 Hz, 1H), 3.91-3.68 (m, 5H), 3.63-3.45 (m, 3H), 3.13 (t, J=11.3 Hz, 3H), 2.71-2.57 (m, 2H), 2.20 (br. s., 2H), 1.98 (br. s., 1H), 1.84 (d, J=10.5 Hz, 1H), 1.65 (br. s., 2H), 1.51 (br. s., 1H). m/z (ESI) 444.2 (M+H)+.

1. concentrationThe reaction was concentrated
2. customtriturated with diethyl ether
3. filtrationfiltered
4. washThe solids were washed with diethyl ether and vacuum
5. customdried overnight