L-Malic Acid → HCID 131732357, compound
Reaction equation
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:39])([F:38])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[C:40]([OH:48])(=[O:47])[C@H:41]([CH2:43][C:44]([OH:46])=[O:45])[OH:42]>>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:38])([F:39])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[C:40]([O-:48])(=[O:47])[C@H:41]([CH2:43][C:44]([O-:46])=[O:45])[OH:42]Participants
3
Conditions
- Temperature
- 5 °C
Procedure
Nilotinib base (0.300 g, 0.57 mmol) was dissolved in TFE (2 mL) at 40° C. to obtain a mixture. The mixture was stirred and added to a solution of L-malic acid (0.038 g, 0.28 mmol) in TFE (1 mL) at 40° C. The resulting solution was stirred for about 2 h and it was subsequently cooled to 5° C. The mixture was kept at 5° C. overnight while stirring and then a sample (1 ml) was taken from the mixture and evaporated to dryness under reduced pressure at 40° C. to give amorphous Nilotinib L-malate as characterized by the powder X-ray diffractogram depicted in FIG. 44.
Workup
- customto obtain a mixture
- stirringThe resulting solution was stirred for about 2 h
- stirringwhile stirring
- customevaporated to dryness under reduced pressure at 40° C.
Sources & evidence
- ORD record
- ord-683edcebda0a42e5894fa5e95c3deff6
- Source dataset
- uspto-grants-2015_01
- Patent number
- US08937082B2
Reaction notes
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