Phosphorus oxychloride → 2-Chloro-3-(4-methoxyphenyl)pyrazine

HRID 267930노트

반응식

HRID 267930 반응식
O[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)=[N:6][CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:18])=O>>[Cl:18][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)=[N:6][CH:5]=[CH:4][N:3]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 1784889683-(4-Methoxyphenyl)pyrazin-2(1H)-one

생성물 1

HCID 131998882-Chloro-3-(4-methoxyphenyl)pyrazine

실험 절차

The 2-hydroxy-3-p-methoxyphenylpyrazine is refluxed (120°-130°C) with excess phosphorus oxychloride under stirring for 3-5 hours. The solution is evaporated to dryness at 50°C in vacuo, cooled, ice is added, then treated with 10% sodium hydroxide solution, extracted with a suitable solvent such as diethyl ether, the ethereal solution washed with water and evaporated. The crude product is crystallized from a suitable solvent such as ethanol to give 2-chloro-3-p-methoxyphenylpyrazine.

후처리

  1. customThe solution is evaporated to dryness at 50°C in vacuo
  2. temperaturecooled
  3. additionice is added
  4. additiontreated with 10% sodium hydroxide solution
  5. extractionextracted with a suitable solvent such as diethyl ether
  6. washthe ethereal solution washed with water
  7. customevaporated
  8. customThe crude product is crystallized from a suitable solvent such as ethanol

출처 및 근거

ORD 기록
ord-43b7ff0974b84d5396923adc3e3a2dd3
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03946009

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