L-Glutamic Acid → HCID 86688190, compound

HRID 1428284Notes

Reaction equation

HRID 1428284 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.[NH2:40][C@H:41]([C:47]([OH:49])=[O:48])[CH2:42][CH2:43][C:44]([OH:46])=[O:45]>>[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.[NH2:40][C@H:41]([C:47]([O-:49])=[O:48])[CH2:42][CH2:43][C:44]([O-:46])=[O:45]

Participants

3

Reactant 2

HCID 33032L-Glutamic AcidHCID 644241Nilotinib

Product 1

HCID 86688190HCID 86688190, compound

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-glutamic acid (0.042 g, 0.28 mmol) in TFE (1 mL) at 40° C. The resulting solution was stirred for about 4 h and subsequently cooled to 5° C. No precipitation was observed upon cooling. The mixture was kept at 5° C. overnight and then a sample (1 ml) was taken from the mixture and evaporated to dryness under reduced pressure at 40° C. to give Nilotinib glutamate form I.

Workup

  1. customto obtain a mixture
  2. stirringThe resulting solution was stirred for about 4 h
  3. customNo precipitation
  4. temperatureupon cooling
  5. customevaporated to dryness under reduced pressure at 40° C.

Sources & evidence

ORD record
ord-1d2b59773f3245d98734fdf252e46bc9
Source dataset
uspto-grants-2015_01
Patent number
US08937082B2

Reaction notes

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