Acetic Acid → 4'-(12-Acetyloxydodecyloxy)biphenyl-4-carboxylic acid ethyl ester

HRID 231016

반응식

HRID 231016 반응식
O.O.O.O.O.[OH-].C[N+](C)(C)C.CN(C=O)C.[C:17]([OH:20])(=[O:19])[CH3:18].[CH2:21]([O:23][C:24]([C:26]1[CH:31]=[CH:30][C:29]([C:32]2[CH:37]=[CH:36][C:35]([O:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50]Br)=[CH:34][CH:33]=2)=[CH:28][CH:27]=1)=[O:25])[CH3:22]>CCOCC>[CH2:21]([O:23][C:24]([C:26]1[CH:31]=[CH:30][C:29]([C:32]2[CH:37]=[CH:36][C:35]([O:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][O:20][C:17](=[O:19])[CH3:18])=[CH:34][CH:33]=2)=[CH:28][CH:27]=1)=[O:25])[CH3:22]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6228DimethylformamideHCID 82620Tetramethylammonium Hydroxide PentahydrateHCID 539084014'-(12-Bromododecyloxy)biphenyl-4-carboxylic acid ethyl ester

생성물 1

HCID 536569284'-(12-Acetyloxydodecyloxy)biphenyl-4-carboxylic acid ethyl ester수율 67%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

60 m moles(10.9 g) of tetramethylammonium hydroxide pentahydrate was added to a DMF solution of 60 m moles(3.6 g) of acetic acid, and stirred for one hour, then 50 m moles(24.5 g) of the above 4'-(12-bromododecyloxy)biphenyl-4-carboxylic acid ethyl ester was added thereto, and stirred for 12 hours. After the reaction, the reaction solution was ether extracted. The extrate was concentrated, and then purified by column chromatography, to obtain 15.7 g of 4'-(12-acetyloxydodecyloxy)biphenyl-4-carboxylic acid ethyl ester [m.p. 80.1°-81.5° C⟧ (yield: 67%)

후처리

  1. stirringstirred for 12 hours
  2. customAfter the reaction
  3. extractionextracted
  4. concentrationThe extrate was concentrated
  5. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-5d549c02b7d2406ca2f303f466140caa
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04844835

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