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2,5-Hexanedione → 89151-79-1

HRID 1576103
ノート
印刷プレビュー

反応式

HRID 1576103 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

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

生成物 1

HCID 2483894989151-79-1

試薬・触媒・溶媒 4

HCID 241Benzene溶媒
HCID 702
Ethanol
溶媒
2 回
HCID 3283Diethyl Ether溶媒
HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-39d35ffd23a9428b9ba068295a953a2d
出典データセット
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03979408

反応ノート

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