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3-(Trifluoromethyl)phenol → 1-(4-bromobutoxy)-3-(trifluoromethyl)benzene

HRID 1156844
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인쇄 미리보기

반응식

HRID 1156844 반응식
[OH-].[Na+].[OH:3][C:4]1[CH:5]=[C:6]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:8][CH:9]=1.[Br:14][CH2:15][CH2:16][CH2:17][CH2:18]Br>C(Cl)Cl>[F:13][C:10]([F:11])([F:12])[C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=1)[O:3][CH2:18][CH2:17][CH2:16][CH2:15][Br:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 73763-(Trifluoromethyl)phenolHCID 80561,4-DibromobutaneHCID 14798Sodium Hydroxide

생성물 1

HCID 128367631-(4-bromobutoxy)-3-(trifluoromethyl)benzene수율 80.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

267 ml of 1.6 N sodium hydroxide solution are added dropwise with stirring at 100° C. within 90 minutes to a mixture of 69.3 g of 3-hydroxybenzotrifluoride and 119 g of 1,4-dibromobutane. The mixture is stirred at this temperature for a further 5 hours and is then allowed to cool. 200 ml of methylene chloride are added, the organic phase is separated off, washed with dilute sodium hydroxide solution, dried over sodium sulfate and concentrated. The residue is distilled in vacuo. 102.6 g of 4-(3-trifluoromethylphenoxy)butyl bromide of b.p. 143° to 144° C. (13 mm Hg=1730 Pa) are obtained.

후처리

  1. temperatureto cool
  2. customthe organic phase is separated off
  3. washwashed with dilute sodium hydroxide solution
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. distillationThe residue is distilled in vacuo

출처 및 근거

ORD 기록
ord-dcd90ae8baa54f1e907abac5f4ae6a66
출처 데이터셋
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04337267

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