Ammonia → 4-Chloro-2-(4-methoxyphenyl)-6-methylpyrimidine

HRID 1082083

反応式

HRID 1082083 の反応式
O[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[N:3]=1.N.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[N:3]=1

参加物

4

反応物 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 178488949HCID 178488949、化合物

生成物 1

HCID 153834554-Chloro-2-(4-methoxyphenyl)-6-methylpyrimidine

実験手順

6.5 g of 4-hydroxy-2-(4-methoxyphenyl)-6-methylpyrimidine prepared in reference example 1 (3) was added to 30 ml of phosphorus oxychloride, and the mixture was refluxed with stirring for 30 minutes. The reaction mixture was cooled and poured into diluted ammonia solution and the precipitated crystals were filtered off. The crystals were dissolved in chloroform. After the chloroform layer was washed twice with water, it was dried with anhydrous magnesium sulfate and was evaporated in vacuo. The residue was crystallized with n-hexane and filtered off. Whereby 5.1 g of crystals was obtained. Melting point is 80° to 81° C.

後処理

  1. temperaturethe mixture was refluxed
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe precipitated crystals were filtered off
  4. dissolutionThe crystals were dissolved in chloroform
  5. washAfter the chloroform layer was washed twice with water, it
  6. dry with materialwas dried with anhydrous magnesium sulfate
  7. customwas evaporated in vacuo
  8. customThe residue was crystallized with n-hexane
  9. filtrationfiltered off

出典と根拠

ORDレコード
ord-c69c4e3abc1f456ebb318ed87e442425
出典データセット
uspto-grants-1996_12
特許番号
US05589477

関連ノート

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