Phosphorus oxychloride → 2-Chloro-4-(4-methoxyphenyl)pyridine

HRID 657663노트

반응식

HRID 657663 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][N+:12]([O-])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.P(Cl)(Cl)([Cl:18])=O>>[Cl:18][C:13]1[CH:14]=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH:10]=[CH:11][N:12]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 576720264-(4-Methoxyphenyl)pyridine 1-oxide

생성물 1

HCID 534408782-Chloro-4-(4-methoxyphenyl)pyridine

실험 절차

A mixture of 4-(4-methoxyphenyl)pyridine 1-oxide (1.68 g) and phosphorus oxychloride (15 mL) is heated under reflux for six hours and concentrated under reduced pressure. Toluene is added and the mixture concentrated under reduced pressure. The residue is dissolved in hot toluene (20 mL) and the organic phase washed with water (twice 10 mL) a saturated aqueous sodium hydrogenocarbonate solution (10 mL), dried over magnesium sulphate and concentrated under reduced pressure to give 1.45 g of 2-chloro-4-(4-methoxyphenyl)pyridine as an orange coloured crystalline material.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for six hours
  3. concentrationconcentrated under reduced pressure
  4. additionToluene is added
  5. concentrationthe mixture concentrated under reduced pressure
  6. dissolutionThe residue is dissolved in hot toluene (20 mL)
  7. washthe organic phase washed with water (twice 10 mL) a saturated aqueous sodium hydrogenocarbonate solution (10 mL)
  8. dry with materialdried over magnesium sulphate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e70382c90c414390892477b9fc30888c
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076329B2

반응 노트

불러오는 중…