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1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → HCID 178474047、化合物

HRID 2414753
ノート
印刷プレビュー

反応式

HRID 2414753 の反応式
C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.C([O:30][C:31](=O)[CH:32]=[C:33]([NH:46][C:47]1[CH:52]=[CH:51][C:50]([NH:53][C:54](=[O:56])[CH3:55])=[CH:49][CH:48]=1)[C:34]1[CH:39]=[CH:38][C:37]([CH:40]2[CH2:45][CH2:44][CH2:43][CH2:42][CH2:41]2)=[CH:36][CH:35]=1)CCC>CCCCCC>[CH:40]1([C:37]2[CH:36]=[CH:35][C:34]([C:33]3[CH:32]=[C:31]([OH:30])[C:52]4[C:47](=[CH:48][CH:49]=[C:50]([NH:53][C:54](=[O:56])[CH3:55])[CH:51]=4)[N:46]=3)=[CH:39][CH:38]=2)[CH2:41][CH2:42][CH2:43][CH2:44][CH2:45]1
参加物反応条件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 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)HCID 69203597HCID 69203597、化合物

生成物 1

HCID 178474047HCID 178474047、化合物

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

反応条件

温度
250 °C

実験手順

1.2 L of Dowtherm A was charged into a 2 L three neck round bottom flask equipped with a condenser, magnetic stirrer, thermocouple, heating mantle with a variable voltage controller, and a nitrogen inlet. The solvent was heated to 250° C. and 3-(4-acetylaminophenylamino)-3-(4-cyclohexylphenyl)-acrylic acid butyl ester 48 g (0.11 moles) was cautiously added in small portions. As portions were added gas was evolved and foaming occurred. Crystals of product began to form and adhere to the sides of the vessel. After all material had been added heating of the mixture was continued for 1 hour. The mixture was then cooled to room temperature and hexane added. A solid product was collected by vacuum filtration and washed with hexane. After drying in a vacuum oven, 35.7 g (90%) of product was recovered.

後処理

  1. customequipped with a condenser, magnetic stirrer
  2. temperaturethermocouple, heating mantle with a variable voltage controller, and a nitrogen inlet
  3. additionAs portions were added gas
  4. customto form
  5. additionAfter all material had been added
  6. temperatureheating of the mixture
  7. temperatureThe mixture was then cooled to room temperature
  8. filtrationA solid product was collected by vacuum filtration
  9. washwashed with hexane
  10. dry with materialAfter drying in a vacuum oven, 35.7 g (90%) of product
  11. customwas recovered

出典と根拠

ORDレコード
ord-da1c9cc887ea489da4dff5a568e3d05b
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06815447B2

反応ノート

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