Methyl Ethyl Ketone → 2,3-Difluoro-4'-(16-hydroxyhexadecyl)oxybiphenyl

HRID 1289393

반응식

HRID 1289393 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][OH:18].[F:19][C:20]1[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=1[C:27]1[CH:32]=[CH:31][C:30]([OH:33])=[CH:29][CH:28]=1.C(=O)([O-])[O-].[K+].[K+].C(C(C)=O)C>O>[F:19][C:20]1[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=1[C:27]1[CH:32]=[CH:31][C:30]([O:33][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][OH:18])=[CH:29][CH:28]=1

참가 물질

6

반응물 4

HCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 275701316-Bromo-1-hexadecanolHCID 189208344-(2,3-Difluorophenyl)phenol

생성물 1

HCID 189208642,3-Difluoro-4'-(16-hydroxyhexadecyl)oxybiphenyl수율 85%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

First, 3 g of 16-bromo-1-hexadecanol, 1.9 g of 2,3-difluoro-4'-hydroxybiphenyl, 2.6 g of potassium carbonate, and 50 ml of methyl ethyl ketone were placed in a 100 ml flask. The reaction mixture was stirred under reflux for 32 hours. The reaction mixture was poured into water, and an organic layer was extracted with ether. The ether 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 3.5 g of 2,3-difluoro-4'-(16-hydroxyhexadecyl)oxybiphenyl (Y: 84%). The compound thus obtained had a purity of 97.4% by GC.

후처리

  1. temperatureunder reflux for 32 hours
  2. extractionan organic layer was extracted with ether
  3. washThe ether 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-1ab70646ede1462fa027cbbea7af28e8
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750213

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