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Benzhydrylamine → HCID 178522801, 화합물

HRID 574655
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HRID 574655 반응식
[OH:1][C:2]1[C:7]([C:8]([OH:10])=O)=[CH:6][N:5]=[C:4]([N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)[N:3]=1.C1N=CN(C(N2C=NC=C2)=O)C=1.[C:28]1([CH:34]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[NH2:35])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.CCN(CC)CC>CN(C=O)C.O>[CH:34]([NH:35][C:8]([C:7]1[C:2]([OH:1])=[N:3][C:4]([N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)=[N:5][CH:6]=1)=[O:10])([C:36]1[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
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참가 물질

7

반응물 4

HCID 7036BenzhydrylamineHCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 178524762HCID 178524762, 화합물

생성물 1

HCID 178522801HCID 178522801, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

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온도
105 °C

실험 절차

4-Hydroxy-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid (1-1-a, 8 g, 38.8 mmol) and CDI (7.24 g, 44.6 mmol) was dissolved in DMF (80 mL), stirred for 45 min at 105° C., then cooled to 77° C. Diphenylmethanamine (9.2 g, 50.4 mmol) and Et3N (5.41 ml, 38.8 mmol) were then added to the solution at 77° C. and the reaction mixture was stirred for 5 h. The resulting mixture was cooled to ambient temperature, diluted with 150 ml of water, extracted with ethyl acetate (3 times 150 ml). The organic phases were combined, washed with brine, dried over anhydrous Na2SO4, purified by recrystillized in EtOH/Et2O (1/10). A yellow solid was obtained as product, 1-1-b, (6.4 g, 45%). 1H NMR (300 MHz, DMSO-d6) δ 6.32-6.34 (d, J=8.4, 1H), 6.50-6.51 (m, 1H), 7.29-7.43 (m, 11H), 7.74 (s, 1H), 8.55-8.58 (m, 2H), 11.77 (s, 1H). LC-MS 372 [MH]+.

후처리

  1. temperaturecooled to 77° C
  2. stirringthe reaction mixture was stirred for 5 h
  3. temperatureThe resulting mixture was cooled to ambient temperature
  4. extractionextracted with ethyl acetate (3 times 150 ml)
  5. washwashed with brine
  6. dry with materialdried over anhydrous Na2SO4
  7. custompurified
  8. customA yellow solid was obtained as product

출처 및 근거

ORD 기록
ord-84a12e12f24d456fac22ed36269f123c
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09034851B2

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