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

HRID 231016

反応式

HRID 231016 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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%)

後処理

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

出典と根拠

ORDレコード
ord-5d549c02b7d2406ca2f303f466140caa
出典データセット
uspto-grants-1989_07
特許番号
US04844835

関連ノート

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