4-Fluorophenol → Quinoxyfen

HRID 1885529노트

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HRID 1885529 반응식
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

참가 물질

5

반응물 2

HCID 97324-FluorophenolHCID 6158354,5,7-Trichloroquinoline

생성물 1

HCID 3391107Quinoxyfen수율 76.4%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 14798Sodium Hydroxide용매

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온도
160 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-feb7b7f5ccc543dba9aba0eda0744e6d
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05145843

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