反应详情

A solution of N-tert-butyl-5-(4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-(hydroxymethyl) pyrimidin-2-yl) thiophene-2-sulfonamide (89 mg, 0.17 mmol, 1.0 eq) and BCl3 (1.0 ml, 1.0 mmol, 6.0 equiv.) in CH2Cl2 (5 mL) was stirred for 1 h at 0° C. After addition od water and extraction with EtOAc (3×50 ml), the combined organic phases were washed (brine), dried (Na2SO4), filtered and concentrated to produce 5-(4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-(hydroxymethyl)pyrimidin-2-yl)thiophene-2-sulfonamide (Compound 171) (50.0 mg, 74.8%) as white solid. LC-MS (m/z)=393.0 [M+H]+; 1H 1H NMR (400 MHz, DMSO-d6): δ 0.75-0.76 (m, 2H), 0.97-0.99 (m, 2H), 1.92-1.96 (m, 1H), 4.56 (d, J=5.2 Hz, 2H), 5.61 (t, J=5.2 Hz, 1H), 6.53 (d, J=10.4 Hz, 1H), 7.58 (d, J=3.6 Hz, 1H), 7.78 (s, 3H), 8.24 (s, 1H), 8.95 (s, 1H), 12.16 (s, 1H).

1. washthe combined organic phases were washed (brine)
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated