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Potassium Hydroxide → HCID 18971052、化合物

HRID 2395201
ノート
印刷プレビュー

反応式

HRID 2395201 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH2:15][CH2:16][C:17]([F:29])([F:28])[C:18]([F:27])([F:26])[C:19]([F:25])([F:24])[C:20]([F:23])([F:22])[F:21])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[OH-:30].[K+]>O1CCCC1>[OH:30][CH2:6][CH2:7][CH2:2][CH2:3][CH2:4][CH2:5][CH2:8][CH2:9][O:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]([O:14][CH2:15][CH2:16][C:17]([F:28])([F:29])[C:18]([F:26])([F:27])[C:19]([F:24])([F:25])[C:20]([F:21])([F:22])[F:23])=[CH:12][CH:13]=2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 22465771HCID 22465771、化合物

生成物 1

HCID 18971052HCID 18971052、化合物収率 67.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In a flask, 1.7 g of 4-hydroxy-4'-[2-(perfluorobutyl)ethyloxy]biphenyl and 10 ml of tetrahydrofuran were placed. To this solution, 3.9 ml of a 1N aqueous solution of potassium hydroxide was added and stirred for a while. After the solvent was distilled away under a reduced pressure, 15 ml of methanol and 0.85 g of 8-bromooctanol were added to the solution and stirred under reflux for 12 hours. Next, the reaction solution was poured into water, and an organic layer was extracted with ether. The ether layer was washed with dilute hydrochloric acid and water in this order. After the solvent was distilled away, the residue was purified by silica gel column chromatography (eluent: benzene/ethyl acetate=9/1), and recrystallized from toluene to give 1.5 g of 4-(8-hydroxyoctyloxy)-4'-[2-(perfluorobutyl)ethyloxy]biphenyl (Y: 67.2%). The purity of the compound thus obtained was 98.8% by GC.

後処理

  1. distillationAfter the solvent was distilled away under a reduced pressure, 15 ml of methanol and 0.85 g of 8-bromooctanol
  2. additionwere added to the solution
  3. stirringstirred
  4. temperatureunder reflux for 12 hours
  5. additionNext, the reaction solution was poured into water
  6. extractionan organic layer was extracted with ether
  7. washThe ether layer was washed with dilute hydrochloric acid and water in this order
  8. distillationAfter the solvent was distilled away
  9. customthe residue was purified by silica gel column chromatography (eluent: benzene/ethyl acetate=9/1)
  10. customrecrystallized from toluene

出典と根拠

ORDレコード
ord-d8e979e009d34053b5fc80f864c38a12
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05814378

反応ノート

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