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2,5-Hexanedione → 89151-79-1

HRID 1576103
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HRID 1576103 반응식
[CH3:1][C:2](=O)[CH2:3][CH2:4][C:5](=O)[CH3:6].I.[NH:10]([C:12]1[NH:13][CH2:14][CH2:15][N:16]=1)[NH2:11].[OH-].[K+].[C:19]([OH:26])(=[O:25])/[CH:20]=[CH:21]\[C:22]([OH:24])=[O:23]>CCOCC.C(Cl)Cl.C1C=CC=CC=1.C(O)C>[C:19]([OH:26])(=[O:25])/[CH:20]=[CH:21]\[C:22]([OH:24])=[O:23].[CH3:1][C:2]1[N:11]([NH:10][C:12]2[NH:16][CH2:15][CH2:14][N:13]=2)[C:5]([CH3:6])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 80352,5-HexanedioneHCID 14797Potassium HydroxideHCID 444266Maleic AcidHCID 122212302-hydrazinyl-4,5-dihydro-1H-imidazole hydroiodide

생성물 1

HCID 2483894989151-79-1

시약·촉매·용매 4

HCID 241Benzene용매
HCID 702
Ethanol
용매
2회
HCID 3283Diethyl Ether용매
HCID 6344Dichloromethane용매

실험 절차

To a boiling solution of 8.63 g. (0.0756 mole) of 2,5-hexanedione in 50 ml. of absolute ethanol, a solution of 14 g. (0.0614 mole) of 2-hydrazino-4,5-dihydro-1H-imidazole hydroiodide and 3.47 g. (0.0620 mole) of potassium hydroxide in 120 ml. of absolute ethanol and 60 ml. of anhydrous benzene is quickly added. The mixture is stirred under reflux for 30 minutes and at room temperature for 12 hours. The potassium iodide which forms is cast off by filtration, then the mixture is concentrated to small volume by evaporating off the solvent. A residue is obtained which is dissolved with methylene chloride. To the obtained solution an ether solution of maleic acid is added and a precipitate readily forms, which is recrystallized two times from absolute ethanol. Yield 1.3 g. M.p. 177°-8°C. The free base melts at 192°-3°C (from methanol.

후처리

  1. filtrationThe potassium iodide which forms is cast off by filtration
  2. concentrationthe mixture is concentrated to small volume
  3. customby evaporating off the solvent
  4. customA residue is obtained which
  5. customwhich is recrystallized two times from absolute ethanol

출처 및 근거

ORD 기록
ord-39d35ffd23a9428b9ba068295a953a2d
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03979408

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