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Cyclohexene → HCID 15650854, 화합물

HRID 1941229
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HRID 1941229 반응식
[CH3:1][C:2]1[C:11]2[O:10][C:9]([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)=[CH:8][C:7](=[O:18])[C:6]=2[CH:5]=[CH:4][C:3]=1[O:19]CC1C=CC=CC=1.C1CCCCC=1>C(OCC)(=O)C.[Pd]>[OH:19][C:3]1[CH:4]=[CH:5][C:6]2[C:7](=[O:18])[CH:8]=[C:9]([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[O:10][C:11]=2[C:2]=1[CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8079CyclohexeneHCID 115954977-(benzyloxy)-8-methyl-2-morpholino-4H-chromen-4-one

생성물 1

HCID 15650854HCID 15650854, 화합물수율 74%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

Part A: 8-Methyl-2-(4-morpholinyl)-7-(phenylmethoxy)-4H-1-benzopyran-4-one (8.59 g, 24.4 mmol.) is suspended in 250 ml of ethyl acetate. 9.9 ml of cyclohexene is added followed by 0.85 g of 10% Palladium on carbon. The mixture is heated at reflux for 18 hours. The reaction is allowed to cool and filtered, the solid is taken up in methanol, decanted and filtered. The methanol is evaporated to give 4.71 g (74%) of the phenol (mp>250° C.).

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후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 18 hours
  3. temperatureto cool
  4. filtrationfiltered
  5. customdecanted
  6. filtrationfiltered
  7. customThe methanol is evaporated

출처 및 근거

ORD 기록
ord-53e48daafc884dacb283e1db2953d2de
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05703075

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