Methyl Ethyl Ketone → 2,3-Difluoro-4'-(11-hydroxyundecyl)oxybiphenyl

HRID 1289376

반응식

HRID 1289376 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.Br[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][OH:28].C(=O)([O-])[O-].[K+].[K+].C(C(C)=O)C>O>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][OH:28])=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 7416311-Bromo-1-undecanolHCID 189208344-(2,3-Difluorophenyl)phenol

생성물 1

HCID 189208442,3-Difluoro-4'-(11-hydroxyundecyl)oxybiphenyl수율 88%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

First, 5.0 g of 2,3-difluoro-4'-hydroxybiphenyl, 7.3 g of 11-bromo-1-undecanol, 6.7 g of potassium carbonate, and 150 ml of methyl ethyl ketone were placed in a 200 ml flask. The mixture was stirred under reflux for 20 hours. The reaction mixture was poured into water and an organic layer was extracted with toluene. The toluene layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was recrystallized from acetone to obtain 8 g of 2,3-difluoro-4'-(11-hydroxyundecyl)oxybiphenyl (Y: 88%). The compound thus obtained had a purity of 98.8% by GC.

후처리

  1. temperatureunder reflux for 20 hours
  2. extractionan organic layer was extracted with toluene
  3. washThe toluene layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThereafter, the solvent was distilled away
  6. customThe residue was recrystallized from acetone

출처 및 근거

ORD 기록
ord-c026200e6b20460c83d86db29ad9d85a
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750213

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