Ethanol → Diethyl diphenate

HRID 132730

反応式

HRID 132730 の反応式
[C:1]12[C:13]3=[CH:14][CH:15]=[CH:16][CH:17]=[C:12]3[C:10](=[O:11])[O:9][C:7](=[O:8])[C:2]1=[CH:3][CH:4]=[CH:5][CH:6]=2.[CH2:18](O)[CH3:19].[C:21]1([CH3:27])C=CC=CC=1.S(=O)(=O)(O)[OH:29]>O>[C:13]1([C:1]2[C:2]([C:7]([O:8][CH2:18][CH3:19])=[O:29])=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:12]([C:10]([O:9][CH2:21][CH3:27])=[O:11])=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 1140TolueneHCID 72794Diphenic anhydride

生成物 1

HCID 13793399Diethyl diphenate収率 90%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 0.1 mol 2,2′-biphenyl dicarboxylic acid anhydride were added 0.3 mol ethanol, 40 ml toluene, and 0.4 ml concentrated sulfuric acid with stirring. Then the reaction mixture was heated refluxing and the water produced was removed by using a water separator until the amount of the water separated reached theoretical value. Upon the reaction completion, the mixture was neutralized with saturated sodium carbonate solution and extracted with ethyl acetate. The upper layer was separated, washed with saturated saline to neutrality, and dried over anhydrous sodium sulfate. The solvent was removed. Distillation under reduced pressure gave diethyl 2,2′-biphenyldicarboxylate as a colorless liquid, and the yield was 90%.

後処理

  1. temperatureThen the reaction mixture was heated
  2. temperaturerefluxing
  3. customwas removed
  4. customseparated
  5. extractionextracted with ethyl acetate
  6. customThe upper layer was separated
  7. washwashed with saturated saline to neutrality
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe solvent was removed
  10. distillationDistillation under reduced pressure

出典と根拠

ORDレコード
ord-8e657e9a56ee4cfabb358574cb2a8f22
出典データセット
uspto-grants-2008_06
特許番号
US07388061B2

関連ノート

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