反应详情

A mixture of N-tert-butyl-5-(4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-vinylpyrimidin-2-yl)thiophene-2-sulfonamide (80 mg, 0.17 mmol) and BCl3 (3 mL) in DCM (10 mL) was stirred for 0.5 h, Water was added and extracted with EA. The combined organic layers were dried (NaHSO4), filtered. The filtrate was concentrated to afford the compound 5-(4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-vinylpyrimidin-2-yl)thiophene-2-sulfonamide (Compound 209) (70 mg, 90%). LC-MS (m/z)=389 [M+H]+; 1H NMR (400 MHz, DMSO-d6): 0.80-0.81 (m, 2H), 1.01-1.04 (m, 2H), 1.96-2.02 (m, 1H), 5.50 (d, J=11.6 Hz, 1H), 5.96 (d, J=17.2 Hz, 1H), 6.43 (s, 1H), 7.08-7.15 (m, 1H), 7.63 (d, J=4 Hz, 1H), 7.87 (bs, 2H), 8.00 (bs, 1H), 8.56 (s, 1H), 10.13 (bs, 1H).

1. extractionextracted with EA
2. dry with materialThe combined organic layers were dried (NaHSO4)
3. filtrationfiltered
4. concentrationThe filtrate was concentrated