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2,5-Bis(2,5-dimethybenzoyl)terephthalic acid → 2,5-Bis(2,5-dimethylbenzyl)terephthalic acid

HRID 488966
ノート
印刷プレビュー

反応式

HRID 488966 の反応式
[CH3:1][C:2]1[CH:31]=[CH:30][C:29]([CH3:32])=[CH:28][C:3]=1[C:4]([C:6]1[CH:14]=[C:13]([C:15]([OH:17])=[O:16])[C:12]([C:18](=O)[C:19]2[CH:24]=[C:23]([CH3:25])[CH:22]=[CH:21][C:20]=2[CH3:26])=[CH:11][C:7]=1[C:8]([OH:10])=[O:9])=O.[H][H]>O1CCCC1.[Pd]>[CH3:1][C:2]1[CH:31]=[CH:30][C:29]([CH3:32])=[CH:28][C:3]=1[CH2:4][C:6]1[CH:14]=[C:13]([C:15]([OH:17])=[O:16])[C:12]([CH2:18][C:19]2[CH:24]=[C:23]([CH3:25])[CH:22]=[CH:21][C:20]=2[CH3:26])=[CH:11][C:7]=1[C:8]([OH:10])=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 225613632,5-Bis(2,5-dimethybenzoyl)terephthalic acidHCID 178418361HCID 178418361、化合物

生成物 1

HCID 222694722,5-Bis(2,5-dimethylbenzyl)terephthalic acid

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
117 °C

実験手順

A mixture of 92 grams of 2,5-bis(2,5-dimethybenzoyl)terephthalic acid in 1.5 L of tetrahydrofuran was treated with 9.2 grams of 10% palladium on carbon (as a catalyst) in an atmosphere of hydrogen at 270 kPa and 65° C. for 17 hours. The reaction mixture was filtered through Celite™ diatomaceous earth filter agent to remove the catalyst. The filtrate was concentrated in vacuo to give a solid. The solid was triturated with ethyl acetate, collected by filtration, and dried. To 75 grams of the solid was added 1250 grams of acetic acid, and the resulting mixture was heated to 117° C. for 30 minutes and cooled to room temperature. The resulting solid was collected by filtration and washed with acetic acid followed by heptane. The resulting residue was dried to give 2,5-bis(2,5-dimethybenzyl)terephthalic acid.

後処理

  1. filtrationThe reaction mixture was filtered through Celite™ diatomaceous earth
  2. filtrationfilter agent
  3. customto remove the catalyst
  4. concentrationThe filtrate was concentrated in vacuo
  5. customto give a solid
  6. customThe solid was triturated with ethyl acetate
  7. filtrationcollected by filtration
  8. customdried
  9. additionTo 75 grams of the solid was added 1250 grams of acetic acid
  10. temperaturecooled to room temperature
  11. filtrationThe resulting solid was collected by filtration
  12. washwashed with acetic acid
  13. customThe resulting residue was dried

出典と根拠

ORDレコード
ord-27ca69c1d650401d86682b54153f6695
出典データセット
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06974877B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート