5-(2,6-Dimorpholinopyrimidin-4-yl)-4-(trifluoromethyl)pyridin-2-amine hydrochloride hydrate → Buparlisib Hydrochloride

HRID 709531Notes

Reaction equation

HRID 709531 reaction equation
[ClH:1].O.[N:3]1([C:9]2[N:14]=[C:13]([C:15]3[C:16]([C:22]([F:25])([F:24])[F:23])=[CH:17][C:18]([NH2:21])=[N:19][CH:20]=3)[CH:12]=[C:11]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)[N:10]=2)[CH2:8][CH2:7][O:6][CH2:5][CH2:4]1>CO>[ClH:1].[N:3]1([C:9]2[N:14]=[C:13]([C:15]3[C:16]([C:22]([F:25])([F:23])[F:24])=[CH:17][C:18]([NH2:21])=[N:19][CH:20]=3)[CH:12]=[C:11]([N:26]3[CH2:27][CH2:28][O:29][CH2:30][CH2:31]3)[N:10]=2)[CH2:4][CH2:5][O:6][CH2:7][CH2:8]1

Participants

3

Reactant 1

HCID 668340295-(2,6-Dimorpholinopyrimidin-4-yl)-4-(trifluoromethyl)pyridin-2-amine hydrochloride hydrate

Product 1

HCID 66577015Buparlisib Hydrochloride

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

40 mg of 5-(2,6-Di-4-morpholinyl-4-pyrimidinyl)-4-(trifluoromethyl)pyridin-2-amine monohydrate monohydrochloride of Example 6 is equilibrated in 0.4 mL methanol in a vial at 25° C.±0.1 for 24 hours equilibration time (with constant agitation). The solution is evaporated to dryness by nitrogen flow at room temperature. The resulting solid is collected prior to complete dryness and examined by X-ray powder diffraction to yield Polymorph Form SE of the monohydrochloride salt of the compound of Formula A.

Workup

  1. customvial at 25° C.
  2. customfor 24 hours
  3. customThe solution is evaporated to dryness by nitrogen flow at room temperature
  4. customThe resulting solid is collected

Sources & evidence

ORD record
ord-2ea875ce67b1470fba2ad4d803f13fff
Source dataset
uspto-grants-2015_11
Patent number
US09181215B2

Reaction notes

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