Potassium Carbonate → 4-[4-(11-Bromo-undecyloxy)-phenyl]-cyclohexanol

HRID 2220003노트

반응식

HRID 2220003 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][CH:5]([C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[Br:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]Br.C([O-])([O-])=O.[K+].[K+]>CC(=O)CC>[Br:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][O:14][C:11]1[CH:10]=[CH:9][C:8]([CH:5]2[CH2:4][CH2:3][CH:2]([OH:1])[CH2:7][CH2:6]2)=[CH:13][CH:12]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 855511,11-DibromoundecaneHCID 101764984-(cis-4-Hydroxycyclohexyl)phenol

생성물 1

HCID 179809754-[4-(11-Bromo-undecyloxy)-phenyl]-cyclohexanol수율 85%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture of 2.40 g (0.012 mol) of 4-(4-Hydroxy-cyclohexyl)-phenol obtained in Step 1, 11.76 (0.037 mol) of 1,11-Dibromoundecane, 5.17 g (0.037 mol) of K2CO3 and 40 mL of dry butanone is refluxed for 24 h, then allowed to return to room temperature. The reaction mixture is filtered off and the butanone is distilled off under reduced pressure. The crude product is purified by recrystallisation from ethanol to give a pure product as a white solid (4.34 g, 85% yield).

후처리

  1. temperatureis refluxed for 24 h
  2. customto return to room temperature
  3. filtrationThe reaction mixture is filtered off
  4. distillationthe butanone is distilled off under reduced pressure
  5. customThe crude product is purified by recrystallisation from ethanol

출처 및 근거

ORD 기록
ord-1f8b331ecbaa47a8af0068c7531042e7
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07416682B2

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