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Phosphorus oxychloride → HCID 22617793, 화합물

HRID 842057
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HRID 842057 반응식
[N+:1]([C:4]1[C:5](=O)[NH:6][C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N:8][CH:9]=1)([O-:3])=[O:2].P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 135216835-Nitro-2-phenylpyrimidin-4(3H)-one

생성물 1

HCID 22617793HCID 22617793, 화합물수율 86%

반응 조건

온도
90 °C

실험 절차

A mixture of 5-nitro-2-phenyl-4(3H)-pyrimidinone (6 g) and phosphorus oxychloride (8.5 g) is stirred at 90° C. for four hours. After cooling, the reaction mixture is concentrated under reduced pressure, and the residue is dissolved in chloroform. To the mixture is added ice-water, and the mixture is stirred. The mixture is neutralized with 1N aqueous sodium hydroxide solution, and the chloroform layer is separated, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue is recrystallized from ethanol to give the desired compound (5.6 g).

후처리

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture is concentrated under reduced pressure
  3. dissolutionthe residue is dissolved in chloroform
  4. additionTo the mixture is added ice-water
  5. stirringthe mixture is stirred
  6. customthe chloroform layer is separated
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-044eb27cac414ad1af908fb183ff90f7
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06372740B1

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