Phosphorus pentachloride → 2-Chloro-5-ethyl-6-methyl-3-nitropyridine

HRID 1033004노트

반응식

HRID 1033004 반응식
[N+:1]([C:4]1[C:5](=O)[NH:6][C:7]([CH3:12])=[C:8]([CH2:10][CH3:11])[CH:9]=1)([O-:3])=[O:2].P(Cl)(Cl)(Cl)(Cl)[Cl:15]>C(Cl)(Cl)Cl>[Cl:15][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][C:8]([CH2:10][CH3:11])=[C:7]([CH3:12])[N:6]=1

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 103523142(1H)-Pyridinone, 5-ethyl-6-methyl-3-nitro-

생성물 1

HCID 103755472-Chloro-5-ethyl-6-methyl-3-nitropyridine수율 67%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
140 °C

실험 절차

A mixture of 3-nitro-5-ethyl-6-methylpyridin-2(1H)-one (0.91 g, 5.0 mmol) and phosphorus pentachloride (1.25 g, 6.0 mmol), under a nitrogen atmosphere, was heated at 140° C. for 0.5 hours. The cooled mixture was diluted with chloroform and ice water. The separated chloroform layer was then washed with water, saturated aqueous NaHCO3 and dried (Na2SO4). After filtering through a pad of charcoal, solvent was evaporated to yield 672 mg (67%) of product.

후처리

  1. washThe separated chloroform layer was then washed with water, saturated aqueous NaHCO3
  2. dry with materialdried (Na2SO4)
  3. filtrationAfter filtering through a pad of charcoal, solvent
  4. customwas evaporated

출처 및 근거

ORD 기록
ord-3861344d06fa41ed90f224e026380e4b
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05308854

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