Hydrochloric Acid → Bavisant dihydrochloride anhydrous
반응식
[CH:1]1([N:4]2[CH2:9][CH2:8][N:7]([C:10]([C:12]3[CH:17]=[CH:16][C:15]([CH2:18][N:19]4[CH2:24][CH2:23][O:22][CH2:21][CH2:20]4)=[CH:14][CH:13]=3)=[O:11])[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.[ClH:25]>C(O)C>[ClH:25].[ClH:25].[CH:1]1([N:4]2[CH2:5][CH2:6][N:7]([C:10]([C:12]3[CH:13]=[CH:14][C:15]([CH2:18][N:19]4[CH2:20][CH2:21][O:22][CH2:23][CH2:24]4)=[CH:16][CH:17]=3)=[O:11])[CH2:8][CH2:9]2)[CH2:3][CH2:2]1참가 물질
4
반응 조건
- 온도
- 60 °C
실험 절차
A 250 mL, three-neck flask fitted with a mechanical stirrer, addition funnel, thermocouple probe, and heating mantle was charged with (4-cyclopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone (11.0 g, 0.034 mol, 1.0 eq) and ethanol (75 mL). The resulting solution was heated to 60° C. Concentrated hydrochloric acid (6.1 mL, 0.074 mol, 2.2 eq) was then added dropwise over 8 min. The reaction mixture was then heated at 60° C. for a further 10 min and then slowly cooled to 20° C. over 3 hrs. The resulting solid was collected by filtration, rinsed with pentane, and dried at 50° C. for 3 hrs in a vacuum oven to yield the title compound as a white solid.