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

HRID 983738
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인쇄 미리보기

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HRID 983738 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 225613632,5-Bis(2,5-dimethybenzoyl)terephthalic acidHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

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온도
117 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-18e76c7683c349338751057cb71fa819
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06864396B2

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