Methyl Ethyl Ketone → 2,3-Difluoro-4'-(6-hydroxyhexyl)oxybiphenyl

HRID 1289385

反応式

HRID 1289385 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][OH:8].[F:9][C:10]1[C:15]([F:16])=[CH:14][CH:13]=[CH:12][C:11]=1[C:17]1[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+].C(C(C)=O)C>O>[F:9][C:10]1[C:15]([F:16])=[CH:14][CH:13]=[CH:12][C:11]=1[C:17]1[CH:22]=[CH:21][C:20]([O:23][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][OH:8])=[CH:19][CH:18]=1

参加物

6

反応物 4

HCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 779706-Bromo-1-hexanolHCID 189208344-(2,3-Difluorophenyl)phenol

生成物 1

HCID 189208402,3-Difluoro-4'-(6-hydroxyhexyl)oxybiphenyl収率 63.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

First, 5 g of 6-bromo-1-hexanol, 5.7 g of 2,3difluoro-4'-hydroxybiphenyl, 7.6 g of potassium carbonate, and 70 ml of methyl ethyl ketone were placed in a 100 ml flask. Then, 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 5.4 g of 2,3-difluoro-4'-(6-hydroxyhexyl)oxybiphenyl (Y: 63.5%). The compound thus obtained had a purity of 99.9% by GC.

後処理

  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

出典と根拠

ORDレコード
ord-be28440a12e4484a887f9ddf837cce26
出典データセット
uspto-grants-1998_05
特許番号
US05750213

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