Phosphorus oxychloride → 2-Chloro-3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine

HRID 4325

반응식

HRID 4325 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[NH:16][C:15](=O)[N:14]([CH3:18])[C:13](=[N:19][C:20]3[C:25]([CH3:26])=[CH:24][C:23]([CH3:27])=[CH:22][C:21]=3[CH3:28])[CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].P(Cl)(Cl)([Cl:31])=O>>[Cl:31][C:15]1[N:14]([CH3:18])[C:13](=[N:19][C:20]2[C:25]([CH3:26])=[CH:24][C:23]([CH3:27])=[CH:22][C:21]=2[CH3:28])[CH:12]=[C:11]([C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[N:16]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178418505HCID 178418505, 화합물

생성물 1

HCID 201522932-Chloro-3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine

실험 절차

To 3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)-2-(1H)pyrimidone (5.0 g) was added phosphorus oxychloride (50 ml). The mixture was refluxed for 7 hours and evaporated under reduced pressure. The resulting syrup was triturated in a mixture of ice and water, neutralized with aqueous sodium bicarbonate and extracted with chloroform. The extract was dried and evaporated under reduced pressure. The residue was chromatographed on silica gel using chloroform to give 2-chloro-3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (3.26 g).

후처리

  1. temperatureThe mixture was refluxed for 7 hours
  2. customevaporated under reduced pressure
  3. customThe resulting syrup was triturated in a mixture of ice and water
  4. extractionextracted with chloroform
  5. customThe extract was dried
  6. customevaporated under reduced pressure
  7. customThe residue was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-53723e478eea4102a066bd715aecef75
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725600

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