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4,6-Dimethylpyrimidin-2-ol → 2-Chloro-4,6-dimethylpyrimidine

HRID 230298
ノート
印刷プレビュー

反応式

HRID 230298 の反応式
P(Cl)(Cl)([Cl:3])=O.[CH3:6][C:7]1[CH:12]=[C:11]([CH3:13])[N:10]=[C:9](O)[N:8]=1.C(=O)([O-])O.[Na+]>O>[Cl:3][C:9]1[N:8]=[C:7]([CH3:6])[CH:12]=[C:11]([CH3:13])[N:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 95084,6-Dimethylpyrimidin-2-olHCID 24813Phosphorus oxychlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 205502-Chloro-4,6-dimethylpyrimidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Under an argon atmosphere, phosphorus oxychloride (2 ml) was added to 4,6-dimethyl-2-hydroxypyrimidine (400 mg), and the resulting mixture was stirred for 1 hour while heating the mixture to reflux. The reaction solution was cooled to room temperature, and the cooled solution was added in small portions to water. After adding sodium hydrogen carbonate in small portions to the resulting mixture to neutralize it, the mixture was extracted with ethyl acetate. Organic layer was washed twice with water and once with saturated brine, and dried over anhydrous sodium sulfate. After removing anhydrous sodium sulfate by filtration, the filtrate was concentrated to obtain 2-chloro-4,6-dimethylpyrimidine (350 mg). (2) In the same manner as in Reference Example 8, 4-iodophenol (223 mg) and 2-chloro-4,6-dimethylpyrimidine (157 mg) were reacted by using sodium hydride to obtain 2-(4-iodophenoxy)-4,6-dimethylpyrimidine (226 mg).

後処理

  1. temperaturewhile heating the mixture
  2. temperatureto reflux
  3. extractionthe mixture was extracted with ethyl acetate
  4. washOrganic layer was washed twice with water and once with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customAfter removing anhydrous sodium sulfate
  7. filtrationby filtration
  8. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-5ccc550426494100875ec5a54fce51f6
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07566724B2

反応ノート

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