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Ethyl Acetate → 3',4'-Didemethylnobiletin

HRID 371409
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HRID 371409 반응식
C(OCC)(=O)C.C([O:14][C:15]1[CH:16]=[C:17]([CH:37]=[CH:38][C:39]=1[O:40]CC1C=CC=CC=1)[C:18]1[O:19][C:20]2[C:25]([C:26](=[O:28])[CH:27]=1)=[C:24]([O:29][CH3:30])[C:23]([O:31][CH3:32])=[C:22]([O:33][CH3:34])[C:21]=2[O:35][CH3:36])C1C=CC=CC=1>[Pd].CO>[OH:14][C:15]1[CH:16]=[C:17]([CH:37]=[CH:38][C:39]=1[OH:40])[C:18]1[O:19][C:20]2[C:25]([C:26](=[O:28])[CH:27]=1)=[C:24]([O:29][CH3:30])[C:23]([O:31][CH3:32])=[C:22]([O:33][CH3:34])[C:21]=2[O:35][CH3:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8857Ethyl AcetateHCID 13469722HCID 13469722, 화합물

생성물 1

HCID 53180413',4'-Didemethylnobiletin

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Into 200 ml. of a mixed solvent of ethyl acetate and methanol at a ratio of 1:1 was dissolved 1.11 g. of 3',4'-bis(benzyloxy)-5,6,7,8-tetramethoxyflavone and added 0.2 to 0.3 g. of 10% palladium-charcoal. The resulting mixture was mixed with shaking in a stream of H2 gas until H2 absorption was completed. After filtering out the catalyst, the obtained filtrate was concentrated. The residue was recrystallized from methanol to give 0.74 g. (97% of the theoretical amount) of the desired compound being a colorless prismatic crystal.

후처리

  1. additionThe resulting mixture was mixed
  2. filtrationAfter filtering out the catalyst
  3. concentrationthe obtained filtrate was concentrated
  4. customThe residue was recrystallized from methanol
  5. customto give 0.74 g

출처 및 근거

ORD 기록
ord-0c6f07addedb4cc88290cb8017113952
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04532254

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