Potassium Carbonate → 4'-(12-Bromododecyloxy)biphenyl-4-carboxylic acid ethyl ester

HRID 2072642ノート

反応式

HRID 2072642 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=2)=[CH:8][CH:7]=1)=[O:5])[CH3:2].[Br:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]Br.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:13]=[CH:14][C:15]([O:18][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][Br:19])=[CH:16][CH:17]=2)=[CH:8][CH:7]=1)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 187661,12-DibromododecaneHCID 4049156Ethyl 4'-hydroxy-4-biphenylcarboxylate

生成物 1

HCID 539084014'-(12-Bromododecyloxy)biphenyl-4-carboxylic acid ethyl ester収率 67%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

An acetone solution of 90 m moles (21.8 g) of the above 4'-hydroxybiphenyl-4-carboxylic acid ethyl ester, 0.15 mole (49.2 g) of 1,12-dibromododecane, and 0.4 mole (55.3 g) of potassium carbonate was refluxed for four hours. The reaction solution was filtered. The filtrate was concentrated, and then purified by column chromatography, to obtain 29.5 g of 4'-(12-bromododecyloxy)biphenyl-4-carboxylic acid ethyl ester [m.p. 88.6°-90.5° C⟧ (yield: 67%)

後処理

  1. filtrationThe reaction solution was filtered
  2. concentrationThe filtrate was concentrated
  3. custompurified by column chromatography

出典と根拠

ORDレコード
ord-6cd3f833963a41e8a6bc92a9831a9762
出典データセット
uspto-grants-1990_04
特許番号
US04913839

反応ノート

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