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HCID 69960253, 화합물 → HCID 18919039, 화합물

HRID 1291405
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HRID 1291405 반응식
C([O:4][C:5]1[CH:33]=[CH:32][C:8]([C:9]([C:11]2[CH:16]=[CH:15][C:14]([CH:17]=[CH:18][C:19]3[N:28]([CH3:29])[C:27](=[O:30])[C:26]4[C:21](=[CH:22][CH:23]=[CH:24][C:25]=4[CH3:31])[N:20]=3)=[CH:13][CH:12]=2)=[O:10])=[CH:7][CH:6]=1)(=O)C>C1COCC1.C(OCC)(=O)C.CO.[Pd]>[CH3:29][N:28]1[C:27](=[O:30])[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][C:25]=2[CH3:31])[N:20]=[C:19]1[CH2:18][CH2:17][C:14]1[CH:15]=[CH:16][C:11]([C:9](=[O:10])[C:8]2[CH:7]=[CH:6][C:5]([OH:4])=[CH:33][CH:32]=2)=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 69960253HCID 69960253, 화합물

생성물 1

HCID 18919039HCID 18919039, 화합물수율 93.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 19895526THF ethyl acetate methanol용매

실험 절차

To a solution of 2-[2-[4-(4-acetoxybenzoyl)phenyl]vinyl]-3,5-dimethyl-4(3H)-quinazolinone (631 mg) in THF-ethyl acetate-methanol (1:1:1) (50 ml) was added 10% Pd/C (50% hydrous) (126 mg) and the mixture was stirred under hydrogen at room temperature for 2 hours. The catalyst was then filtered off and the filtrate was concentrated. After the residue was suspended in ethanol (10 ml), 1N-aqueous sodium hydroxide solution (2.9 ml) was added and the mixture was stirred at room temperature for 2 hours. This reaction mixture was concentrated and the residue was suspended in water (20 ml) and neutralized with 1N-hydrochloric acid (2.9 ml). The precipitate was collected by filtration, washed with water, and dried to provide 538 mg of white powder.

후처리

  1. filtrationThe catalyst was then filtered off
  2. concentrationthe filtrate was concentrated
  3. addition1N-aqueous sodium hydroxide solution (2.9 ml) was added
  4. stirringthe mixture was stirred at room temperature for 2 hours
  5. concentrationThis reaction mixture was concentrated
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-62f49d39a85b48f1aecc12a5a26a74d8
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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