Phosphoric Acid → HCID 117737666、化合物
反応式
[C:1]([CH:5]1[CH2:10][CH2:9][N:8]([CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C@H:18]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:19]([F:22])([F:21])[F:20])=[CH:14][CH:13]=2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[P:28](=[O:32])([OH:31])([OH:30])[OH:29]>CC(C)=O>[P:28]([OH:32])([OH:31])([OH:30])=[O:29].[C:1]([CH:5]1[CH2:6][CH2:7][N:8]([CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C@H:18]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:19]([F:22])([F:21])[F:20])=[CH:14][CH:13]=2)[CH2:9][CH2:10]1)([CH3:4])([CH3:2])[CH3:3]参加物
4
反応条件
- 温度
- 55 °C
実験手順
Add a 40 mg/mL solution of N-[(1S)-1-{4-[(4-tert-butylpiperidin-1-yl)methyl]phenyl}-2,2,2-trifluoroethyl]methanesulfonamide (0.25 mL) in acetone to a Freeslate CM3 Crystallizer master slurry plate. Dry under nitrogen. Seal Master plate and run on Freeslate CM3 Crystallizer using the Symyx 8.0.3.351 workflow (Add 0.25M phosphoric acid (1.2 mmol), tumble-stir for 90 minutes at 55° C. Filter the mixture and add 2-propanol (800 uL). Evaporate under nitrogen at ambient temperature to give crystals of N-[(1S)-1-{4-[(4-tert-butylpiperidin-1-yl)methyl]phenyl}-2,2,2-trifluoroethyl]methanesulfonamide phosphate.