Toluene → HCID 131713380, 화합물

HRID 1388248노트

반응식

HRID 1388248 반응식
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]

참가 물질

5

반응물 4

HCID 1140TolueneHCID 7237O-XyleneHCID 8371ChloranilHCID 20470557HCID 20470557, 화합물

생성물 1

HCID 131713380HCID 131713380, 화합물

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9bef4165fb134bdc9e8d48dc3e9c7a30
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04431564

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