Phosphoric Acid → HCID 49857753, compound

HRID 705510Notes

Reaction equation

HRID 705510 reaction equation
[N:1]1([C:6]2[CH:7]=[C:8]3[C:13](=[CH:14][CH:15]=2)[N:12]=[C:11]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:10]=[CH:9]3)[CH:5]=[CH:4][N:3]=[CH:2]1.[P:22](=[O:26])([OH:25])([OH:24])[OH:23]>CCO>[P:22]([OH:26])([OH:25])([OH:24])=[O:23].[N:1]1([C:6]2[CH:7]=[C:8]3[C:13](=[CH:14][CH:15]=2)[N:12]=[C:11]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:10]=[CH:9]3)[CH:5]=[CH:4][N:3]=[CH:2]1

Participants

4

Reactant 2

HCID 1004Phosphoric AcidHCID 248987326-(1H-Imidazol-1-yl)-2-phenylquinazoline

Product 1

HCID 49857753HCID 49857753, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

6-(1H-Imidazol-1-yl)-2-phenylquinazoline, 275 mg (1 mmol), is dissolved in EtOH (15 mL) at reflux, 100 mg (1 mmol) of phosphoric acid are added, the mixture is stirred for 30 min., and is then allowed to cool to room temperature and left to stand for 3 days while allowing the solution to evaporate slowly, and the resulting material is filtered and dried at 30° C., 20 mmHg, for 8 hours. 270 mg of product are obtained, XRPD: Form A. TGA: no weight loss up to 250° C. Calculated for C17H12N4.H3PO4: C, 48.59; H, 4.13; N, 15.84. found: C, 57.22; H, 4.22; N, 15.84; H-NMR (d6-DMSO) δ: 9.72 (s, 1H), 8.60-8.50 (m, 2H), 8.48 (d, 1H), 8.41 (d, 1H), 8.23 (d, 1H), 8.21 (s, 1H), 7.98-7.58 (m, 3H), 7.22 (s, 1H).

Workup

  1. temperatureat reflux
  2. waitleft
  3. waitto stand for 3 days
  4. customto evaporate slowly
  5. filtrationthe resulting material is filtered
  6. customdried at 30° C.
  7. wait20 mmHg, for 8 hours

Sources & evidence

ORD record
ord-daf29b00ca194b24b6875fb9b58906d0
Source dataset
uspto-grants-2015_11
Patent number
US09174966B2

Reaction notes

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