Phosphorus oxychloride → 4,5-Dimethyl-6-chloro-2-(4-methylphenyl)pyrimidine

HRID 1077835노트

반응식

HRID 1077835 반응식
[CH3:1][C:2]1[C:3](=O)[NH:4][C:5]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)=[N:6][C:7]=1[CH3:8].P(Cl)(Cl)([Cl:19])=O>>[CH3:8][C:7]1[C:2]([CH3:1])=[C:3]([Cl:19])[N:4]=[C:5]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)[N:6]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 1357047395,6-dimethyl-2-(4-methylphenyl)-3H-pyrimidin-4-one

생성물 1

HCID 194302834,5-Dimethyl-6-chloro-2-(4-methylphenyl)pyrimidine

실험 절차

A mixture of 5,6-dimethyl-2-(4-methylphenyl)-3H-pyrimidin-4-one (6 g) and phosphorus oxychloride (40 ml) was refluxed for 2 hours. Excess phosphorus oxychloride was removed under reduced pressure, ice added to the residue, and the mixture extracted with methylene chloride, the organic layer washed with brine, dried over sodium sulfate, the solvent evaporated under reduced pressure, to yield 6.2 g of 4,5-dimethyl-6-chloro-2-(4-methylphenyl)pyrimidine, m.p. 165° C.

후처리

  1. temperaturewas refluxed for 2 hours
  2. customExcess phosphorus oxychloride was removed under reduced pressure, ice
  3. additionadded to the residue
  4. extractionthe mixture extracted with methylene chloride
  5. washthe organic layer washed with brine
  6. dry with materialdried over sodium sulfate
  7. customthe solvent evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-889be9c1327f49c98791498eed318eb0
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05545645

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