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Diphenyl Ether → HCID 178474047、化合物

HRID 1394114
ノート
印刷プレビュー

反応式

HRID 1394114 の反応式
C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.C1(OC2C=CC=CC=2)C=CC=CC=1.C([O:43][C:44](=O)[CH:45]=[C:46]([NH:59][C:60]1[CH:65]=[CH:64][C:63]([NH:66][C:67](=[O:69])[CH3:68])=[CH:62][CH:61]=1)[C:47]1[CH:52]=[CH:51][C:50]([CH:53]2[CH2:58][CH2:57][CH2:56][CH2:55][CH2:54]2)=[CH:49][CH:48]=1)CCC>CCCCCC>[CH:53]1([C:50]2[CH:49]=[CH:48][C:47]([C:46]3[CH:45]=[C:44]([OH:43])[C:65]4[C:60](=[CH:61][CH:62]=[C:63]([NH:66][C:67](=[O:69])[CH3:68])[CH:64]=4)[N:59]=3)=[CH:52][CH:51]=2)[CH2:54][CH2:55][CH2:56][CH2:57][CH2:58]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7583Diphenyl EtherHCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)2 回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

実験手順

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, was charged 1.2 L of Dowtherm A (a eutectic mixture of 26.5% diphenyl and 73.5% diphenyl oxide). The Dowtherm A was then preheated to 250° C. To this was cautiously added in small portions 48 g (0.11 moles) of 3-(4-acetylamino-phenylamino)-3-(4-cyclohexylphenyl)-acrylic acid butyl ester. As portions were added gas was evolved and foaming occurred. Crystals of product begin to form and adhere to the sides. After all the material had been added the heating of the reaction was continued for 1 hour. The mixture was then cooled to room temperature and hexane was added. The 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. customInto a 2 L three-neck round-bottom flask equipped with a condenser, magnetic stirrer
  2. temperaturethermocouple, heating mantle with a variable voltage controller, and a nitrogen inlet
  3. customwas then preheated to 250° C
  4. additionAs portions were added gas
  5. customto form
  6. additionAfter all the material had been added the
  7. temperatureheating of the reaction
  8. filtrationThe 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-690039b2afac416bb3a5baea50585651
出典データセット
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07348340B2

反応ノート

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