反应详情

温度

-10 °C

To a solution of (+)-N-(t-butyloxy)-1-(4-methoxybenzenesulfonyl)-2-piperazinecarboxamide (30 mg, in dichloroethane is added ethanol (1 drop). The solution is cooled to -10° C. and hydrogen chloride gase is bubbled through for 5 minutes. The reaction is then sealed and stirred for 24 hours at which time the volume is reduced to 1/3 by evaporation and the precipitated solids are filtered and dried (in vacuo) to give (+)-N-hydroxy-1-(4-methoxybenzenesulfonyl)-2-piperazinecarboxamide hydrochloride as a white solid. Melting point 167° C. (dec.). Mass spectrum (thermospray): m/Z 343 (m+1 100%). 1H NMR (CD3OD, 250 MHz, ppm): δ7.76 (d, J=8.9 Hz, 2 H), 7.07 (d, J=8.9 Hz, 2 H), 3.87 (bs, H2O ), 4.19 (d, J=3.3 Hz, 1 H), 3.87 (s, 3 H), 3.58 (bd, J=6.2 Hz, 1 H), 3.42 (bd, J=6.1 Hz, 1 H), 3.30 (bs, CD3OD), 3.16 (d, J=13.5 Hz, 1 H), 2.87 (bd, J=13.3 Hz, 1 H), 2.69 (dd, J=13.3, 3.0 Hz, 1 H), 2.51 (dt, J=12.5, 3.8 Hz, 1 H).

1. customhydrogen chloride gase is bubbled through for 5 minutes
2. customThe reaction is then sealed
3. customis reduced to 1/3 by evaporation
4. filtrationthe precipitated solids are filtered
5. customdried (in vacuo)