Acetic Acid → HCID 86688195, compound

HRID 1428298Notes

Reaction equation

HRID 1428298 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:43])(=[O:42])[CH3:41]>>[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-:43])(=[O:42])[CH3:41]

Participants

3

Reactant 2

HCID 176Acetic AcidHCID 644241Nilotinib

Product 1

HCID 86688195HCID 86688195, compound

Conditions

Temperature
5 °C

Procedure

A solution of Nilotinib base (0.5 g, 0.94 mmol) in glacial acetic acid (2 mL, 4V) was stirred at 40° C. for 5 h. The clear yellow solution was then cooled to 5° C. and maintained at that temperature for 72 h. The mixture was then allowed to warm up to room temperature over a period of 1 h. A solid precipitate formed and was separated by filtration to give Nilotinib acetate form III.

Workup

  1. temperaturemaintained at that temperature for 72 h
  2. temperatureto warm up to room temperature over a period of 1 h
  3. customA solid precipitate formed
  4. customwas separated by filtration

Sources & evidence

ORD record
ord-4aa909bf5600453facd9128409020550
Source dataset
uspto-grants-2015_01
Patent number
US08937082B2

Reaction notes

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