3,4-Dinitrophenol → 4-(3,4-Dinitrophenoxy)-pyridine

HRID 491579노트

반응식

HRID 491579 반응식
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.[N+:8]([C:11]1[CH:12]=[C:13]([OH:20])[CH:14]=[CH:15][C:16]=1[N+:17]([O-:19])=[O:18])([O-:10])=[O:9].Cl.O1CCOCC1.[OH-].[Na+]>CCOC(C)=O.Cl.O>[N+:8]([C:11]1[CH:12]=[C:13]([CH:14]=[CH:15][C:16]=1[N+:17]([O-:19])=[O:18])[O:20][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1)([O-:10])=[O:9]

참가 물질

7

반응물 4

HCID 113483,4-DinitrophenolHCID 122884-ChloropyridineHCID 14798Sodium HydroxideHCID 204431481,4-Dioxane hydrochloride

생성물 1

HCID 177560774-(3,4-Dinitrophenoxy)-pyridine

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 21885828Hydrate;hydrochloride용매

반응 조건

온도
145 °C

실험 절차

4-Chloropyridine (3.20 g, 28.2 mmol) and 3,4-dinitrophenol (5.96 g, 32.4 mmol) were combined in an open round-bottom flask fitted with running water condenser. The reaction flask was heated to 145° C. After 45 min, 4N HCl/dioxane (2.1 mL) was added. The reaction was heated for an additional 25 min then cooled to RT. The mix was dissolved in EtOAc and 0.5 N HCl/water. The aqueous layer was basified with 6 N NaOH. A beige solid was isolated and identified as title compound.

후처리

  1. customfitted with running water condenser
  2. temperatureThe reaction was heated for an additional 25 min
  3. temperaturethen cooled to RT
  4. customA beige solid was isolated

출처 및 근거

ORD 기록
ord-3d9ce4d4a5ba4a3f8afc630eaf4acf43
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531553B2

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