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Phosphoric Acid → HCID 49857753, 화합물

HRID 705510
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HRID 705510 반응식
[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
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참가 물질

4

반응물 2

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

생성물 1

HCID 49857753HCID 49857753, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-daf29b00ca194b24b6875fb9b58906d0
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174966B2

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