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Dimethylformamide → HCID 178433892, 화합물

HRID 555608
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HRID 555608 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:15]([OH:16])=[CH:14][C:13]([CH3:17])=[N:12]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].P(Cl)(Cl)(Cl)=O.CN(C)[CH:25]=[O:26]>>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C:15]([OH:16])=[C:14]([CH:25]=[O:26])[C:13]([CH3:17])=[N:12]2)=[CH:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2]
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참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 178429256HCID 178429256, 화합물

생성물 1

HCID 178433892HCID 178433892, 화합물수율 70%

반응 조건

온도
100 °C

실험 절차

1.89 g (9.33 mmol) of 1-(4-tert-butylphenyl)-5-hydroxy-3-methyl-1H-pyrazole was dissolved in 3.6 ml of dry dimethylformamide, and 1.05 ml (11.26 mmol) phosphorus oxychloride was added gradually at 20° C. or below under cooling with ice. After the addition, the mixture was heated at 100° C. for 3 hours, then cooled to room temperature and poured into 30 ml of ice-cold water. The mixed solution was stirred at room temperature for 18 hours, and the precipitated solid was collected by filtration, washed with 20 ml of water and dried to obtain 1.61 g of the above-identified desired product as a yellow solid (yield 70%).

후처리

  1. temperatureunder cooling with ice
  2. additionAfter the addition
  3. temperaturecooled to room temperature
  4. filtrationthe precipitated solid was collected by filtration
  5. washwashed with 20 ml of water
  6. customdried

출처 및 근거

ORD 기록
ord-9788b77102954d5598b2c9497e32e4fa
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08053453B2

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