Ethanol → 4-(4-Pentenoxy)-4'-nitrobiphenyl

HRID 1193459

反応式

HRID 1193459 の反応式
C(O)C.[OH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=2)=[CH:7][CH:6]=1.[OH-].[K+].Br[CH2:23][CH2:24][CH2:25][CH:26]=[CH2:27]>O>[CH2:27]([O:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=2)=[CH:9][CH:10]=1)[CH2:26][CH2:25][CH:24]=[CH2:23]

参加物

6

反応物 4

HCID 702EthanolHCID 14797Potassium HydroxideHCID 707041-Pentene, 5-bromo-HCID 1380784-Hydroxy-4'-nitrobiphenyl

生成物 1

HCID 199012844-(4-Pentenoxy)-4'-nitrobiphenyl

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 400 ml ethanol is added 21.5 g of 4-hydroxy-4'nitrobiphenyl, and the mixture heated to reflux. A solution of 7.1 g KOH in 30 ml of water is added dropwise at reflux temperatures. After complete addition, 18 g of 5-bromo-1-pentene is added and the reaction medium is heated at reflux temperature for about 15 hours. Ethanol is removed under vacuum from the cooled mixture, and the solid residue is slurried with water in a blender, filtered, washed with water, and air dried. The product then is recrystallized from 90/10 hexane/toluene, mp 74°-76° C.

後処理

  1. temperaturethe mixture heated to reflux
  2. temperatureat reflux temperatures
  3. additionis added
  4. temperaturethe reaction medium is heated
  5. temperatureat reflux temperature for about 15 hours
  6. customEthanol is removed under vacuum from the cooled mixture
  7. filtrationfiltered
  8. washwashed with water, and air
  9. customdried
  10. customThe product then is recrystallized from 90/10 hexane/toluene, mp 74°-76° C.

出典と根拠

ORDレコード
ord-da7580f119a24001b8b72f67536987e9
出典データセット
uspto-grants-1989_03
特許番号
US04810338

関連ノート

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