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

HRID 491579ノート

反応式

HRID 491579 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21885828Hydrate;hydrochloride溶媒

反応条件

温度
145 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3d9ce4d4a5ba4a3f8afc630eaf4acf43
出典データセット
uspto-grants-2009_05
特許番号
US07531553B2

反応ノート

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