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

HRID 1910807

반응식

HRID 1910807 반응식
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

참가 물질

3

반응물 2

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

생성물 1

HCID 205502-Chloro-4,6-dimethylpyrimidine수율 56.1%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7653f81e76fb4780ad016929ecb9e0e0
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08604029B2

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