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

HRID 4325

反応式

HRID 4325 の反応式
[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

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178418505HCID 178418505、化合物

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-53723e478eea4102a066bd715aecef75
出典データセット
uspto-grants-1988_02
特許番号
US04725600

関連ノート

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