Toluene → HCID 131713380、化合物

HRID 1388248ノート

反応式

HRID 1388248 の反応式
C(OCCC1C=CC([C:14]2[CH2:19][CH2:18][CH:17]([C:20]3[CH:25]=[CH:24][C:23]([Br:26])=[CH:22][CH:21]=3)[CH2:16][CH:15]=2)=CC=1)CCC.C1(Cl)[C:33](=[O:34])[C:32](Cl)=[C:31](Cl)[C:29](=O)C=1Cl.[C:39]1(C)C(C)=CC=CC=1.[C:47]1([CH3:53])[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1>>[CH2:33]([O:34][CH2:39][CH2:53][C:47]1[CH:52]=[CH:51][C:50]([C:16]2[C:17]([C:20]3[CH:25]=[CH:24][C:23]([Br:26])=[CH:22][CH:21]=3)=[CH:18][CH:19]=[CH:14][CH:15]=2)=[CH:49][CH:48]=1)[CH2:32][CH2:31][CH3:29]

参加物

5

反応物 4

HCID 1140TolueneHCID 7237O-XyleneHCID 8371ChloranilHCID 20470557HCID 20470557、化合物

生成物 1

HCID 131713380HCID 131713380、化合物

実験手順

A mixture of 1-[p-(β-butyloxyethyl)-phenyl]-4-(p-bromophenyl)-cyclohexene (XV) (55 g, 0.13 mol) obtained in Step H, chloranil (78.4 g, 0.32 mol) and xylene (624 ml) was heated and placed under reflux for 24 hours. After cooling, toluene (800 ml) was added, insoluble solid filtered off and toluene removed by concentrating the filtrate. The resulting raw crystals were recrystallized from ethyl acetate (50 ml) to obtain 4"-(β-butyloxyethyl)-4-bromoterphenyl (XV1) (29 g) having a melting point of 225.7°~227.0° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 24 hours
  3. temperatureAfter cooling
  4. filtrationinsoluble solid filtered off
  5. customtoluene removed
  6. concentrationby concentrating the filtrate
  7. customThe resulting raw crystals were recrystallized from ethyl acetate (50 ml)

出典と根拠

ORDレコード
ord-9bef4165fb134bdc9e8d48dc3e9c7a30
出典データセット
uspto-grants-1984_02
特許番号
US04431564

反応ノート

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