Toluene → 2-Methylbutyl 4-[p-(7-octenyloxy)benzoyloxy]biphenyl-4-carboxylate

HRID 6322

반응식

HRID 6322 반응식
C1(C)C=CC=CC=1.[CH2:8]([O:16][C:17]1[CH:25]=[CH:24][C:20]([C:21]([OH:23])=[O:22])=[CH:19][CH:18]=1)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:14]=[CH2:15].O[C:27]1[CH:32]=[CH:31][C:30]([C:33]2[CH:38]=[CH:37][C:36]([C:39]([O:41][CH2:42][CH:43]([CH3:46])[CH2:44][CH3:45])=[O:40])=[CH:35][CH:34]=2)=[CH:29][CH:28]=1>N1C=CC=CC=1>[CH2:8]([O:16][C:17]1[CH:18]=[CH:19][C:20]([C:21]([O:23][C:36]2([C:39]([O:41][CH2:42][CH:43]([CH3:46])[CH2:44][CH3:45])=[O:40])[CH:35]=[CH:34][C:33]([C:30]3[CH:31]=[CH:32][CH:27]=[CH:28][CH:29]=3)=[CH:38][CH2:37]2)=[O:22])=[CH:24][CH:25]=1)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:14]=[CH2:15]

참가 물질

5

반응물 3

HCID 1140Toluene2회HCID 139075372-Methylbutyl 4'-hydroxybiphenyl-4-carboxylateHCID 139976794-(7-Octenyloxy)benzoic acid2회

생성물 1

HCID 675687822-Methylbutyl 4-[p-(7-octenyloxy)benzoyloxy]biphenyl-4-carboxylate수율 45%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

9 g of p-(7-octenyloxy)benzoic acid obtained in 15.(1) was suspended in toluene, and the suspension was cooled in an ice bath. Added dropwise thereto was 6 g of thionyl chloride. After conclusion of the dropping, the temperature was raised and reaction was carried out for 6 hours at 80° C. After conclusion of the reaction, the reaction solution was concentrated under reduced pressure, to obtain an acid chloride compound. Toluene was added to the acid chloride compound, and the resulting toluene solution was cooled in an ice bath. A toluene solution containing 10 g of 2-methylbutyl 4'-hydroxybiphenyl-4-carboxylate and 3 g of pyridine was added dropwise into the above-described toluene solution of the acid chloride compound. After conclusion of dropping, the temperature was raised, and reaction was carried out for 8 hours at 50° C. After conclusion of the reaction, the product was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethanol, to obtain 8.2 g of the objective ester compound. (Yield: 45%)

후처리

  1. temperaturethe temperature was raised
  2. customreaction
  3. customAfter conclusion of the reaction
  4. washthe product was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-de7405e7ac6843299a46eac854633c2b
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05248446

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