4-Fluorophenol → Quinoxyfen

HRID 2255428ノート

反応式

HRID 2255428 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([Cl:13])=[CH:9][C:10]=2[Cl:12])[N:5]=[CH:4][CH:3]=1.[F:14][C:15]1[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][CH:16]=1>C(OCC)(=O)C.[OH-].[Na+]>[Cl:12][C:10]1[CH:9]=[C:8]([Cl:13])[CH:7]=[C:6]2[C:11]=1[C:2]([O:21][C:18]1[CH:19]=[CH:20][C:15]([F:14])=[CH:16][CH:17]=1)=[CH:3][CH:4]=[N:5]2

参加物

5

反応物 2

HCID 97324-FluorophenolHCID 6158354,5,7-Trichloroquinoline

生成物 1

HCID 3391107Quinoxyfen収率 76.4%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 14798Sodium Hydroxide溶媒

反応条件

温度
160 °C

実験手順

A mixture of 29.11 g of 4,5,7-trichloroquinoline and 16.84 g of 4-fluorophenol was heated to 160° C. After approximately 40 minutes, the molten solution solidified. The solid was dissolved in ethyl acetate and 2N NaOH. The organic layer was washed with base to remove excess phenol, then dried. Solvent was removed by reducing pressure, and the residue was purified by recrystallizing in heptane to produce 29.49 g of the title product. M.P. 105°-106° C.

後処理

  1. washThe organic layer was washed with base
  2. customto remove excess phenol
  3. customdried
  4. customSolvent was removed
  5. customthe residue was purified
  6. customby recrystallizing in heptane

出典と根拠

ORDレコード
ord-070086f1772e493ba15c826b7bd9e346
出典データセット
uspto-grants-1993_08
特許番号
US05240940

反応ノート

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