HCID 46186926, compound → HCID 87330609, compound

HRID 1685211Notes

Reaction equation

HRID 1685211 reaction equation
[CH3:1][N:2]([CH3:37])[CH2:3][CH2:4][N:5]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[C:12]([C:17]([F:20])([F:19])[F:18])[CH:11]=2)[N:7]=[C:6]1[CH:21]1[CH2:26][CH2:25][N:24]([C:27]2[C:28]3[CH2:35][C:34](=[O:36])[NH:33][C:29]=3[N:30]=[CH:31][N:32]=2)[CH2:23][CH2:22]1>CC(O)C.O>[OH2:36].[CH3:1][N:2]([CH3:37])[CH2:3][CH2:4][N:5]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[C:12]([C:17]([F:18])([F:19])[F:20])[CH:11]=2)[N:7]=[C:6]1[CH:21]1[CH2:26][CH2:25][N:24]([C:27]2[C:28]3[CH2:35][C:34](=[O:36])[NH:33][C:29]=3[N:30]=[CH:31][N:32]=2)[CH2:23][CH2:22]1.[CH3:37][N:2]([CH2:3][CH2:4][N:5]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[C:12]([C:17]([F:18])([F:19])[F:20])[CH:11]=2)[N:7]=[C:6]1[CH:21]1[CH2:22][CH2:23][N:24]([C:27]2[C:28]3[CH2:35][C:34](=[O:36])[NH:33][C:29]=3[N:30]=[CH:31][N:32]=2)[CH2:25][CH2:26]1)[CH3:1]

Participants

3

Reactant 1

HCID 46186926HCID 46186926, compound

Product 1

HCID 87330609HCID 87330609, compound

Reagents, catalysts & solvents 1

HCID 21889133Propan-2-ol--water (1/1)Solvent

Procedure

To a 20 mL scintillation vial fitted with stir bar charge with 211 mg of 4-{4-[1-(2-dimethylamino-ethyl)-4-(4-fluoro-3-trifluoromethyl-phenyl)-1H-imidazol-2-yl]piperidin-1-yl}-5,7-dihydro-pyrrolo[2,3-d]-pyrimidin-6-one, followed by 2 mL of a 3:1 IPA/H2O solvent mixture. Seed the suspension with 12 mg of hemihydrate seed crystals (see preparation below). Stir (˜600 RPM) at RT for approximately 4 days. Isolate the product by vacuum filtration.

Workup

  1. customTo a 20 mL scintillation vial fitted
  2. stirringStir (˜600 RPM) at RT for approximately 4 days
  3. customIsolate the product
  4. filtrationby vacuum filtration

Sources & evidence

ORD record
ord-1a500d3990c6456087d241f6d585a4b0
Source dataset
uspto-grants-2012_04
Patent number
US08148387B2

Reaction notes

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