Phosphorus oxychloride → 2-Chloro-4,6-dimethylpyrimidine

HRID 1910807

反応式

HRID 1910807 の反応式
Cl.[CH3:2][C:3]1[CH:8]=[C:7]([CH3:9])[NH:6][C:5](=O)[N:4]=1.O=P(Cl)(Cl)[Cl:13]>>[Cl:13][C:5]1[N:4]=[C:3]([CH3:2])[CH:8]=[C:7]([CH3:9])[N:6]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 123431664,6-Dimethyl-2(1H)-pyrimidinone hydrochloride

生成物 1

HCID 205502-Chloro-4,6-dimethylpyrimidine収率 56.1%

実験手順

A suspension of 4,6-dimethyl-1H-pyrimidin-2-one hydrochloride (3.0 g, 18.75 mmol) in dry POCl3 (25 mL, 272 mmol) was refluxed for 18 hours. The reaction mixture was evaporated to dryness and the residue dissolved in dichloromethane. The solution was washed with sodium bicarbonate solution until the pH of the aqueous washings were neutral, then with brine, dried over anhydrous sodium sulfate, filtered and concentrated under vacuum to afford 2-chloro-4,6-dimethyl-pyrimidine (1.5 g, 56%) as a solid.

後処理

  1. temperaturewas refluxed for 18 hours
  2. customThe reaction mixture was evaporated to dryness
  3. dissolutionthe residue dissolved in dichloromethane
  4. washThe solution was washed with sodium bicarbonate solution until the pH of the aqueous washings
  5. dry with materialwith brine, dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-7653f81e76fb4780ad016929ecb9e0e0
出典データセット
uspto-grants-2013_12
特許番号
US08604029B2

関連ノート

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