Ethanol → HCID 178418414、化合物

HRID 583551

反応式

HRID 583551 の反応式
[H-].[Na+].Cl.[C:4]([NH2:10])(=[NH:9])[CH2:5][CH2:6][CH2:7][CH3:8].[CH:11]([CH:13]=[CH:14][C:15]([O:17][CH3:18])=[O:16])=O.[CH2:19](O)C>C1C=CC=CC=1>[CH2:5]([C:4]1[NH:9][CH:11]=[C:13]([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[N:10]=1)[CH2:6][CH2:7][CH3:8]

参加物

6

反応物 4

HCID 702EthanolHCID 24758Sodium hydrideHCID 111293Methyl 4-oxobut-2-enoateHCID 11615174Pentanimidamide Hydrochloride

生成物 1

HCID 178418414HCID 178418414、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Sodium hydride (2.82 g, 0.117 mol) was dissolved in 30 ml of absolute ethanol at 0° C. Valeramidine hydrochloride (16.71 g, 0.123 mol) was added to this solution, and after 15 minutes the solution was filtered and the collected solid was washed with 20 ml of ethanol and 50 ml of benzene. The combined filtrates were diluted with 750 ml of benzene, 15 g (0.117 mol) of methyl 3-formylacrylate was added, and the mixture was refluxed for 18.5 h using a trap to remove water. The solvents were removed under vacuum and the residue slurried in ether. Evaporation of the ether solution gave the title compound as an oil.

後処理

  1. filtrationafter 15 minutes the solution was filtered
  2. washthe collected solid was washed with 20 ml of ethanol and 50 ml of benzene
  3. additionwas added
  4. temperaturethe mixture was refluxed for 18.5 h
  5. customto remove water
  6. customThe solvents were removed under vacuum
  7. customEvaporation of the ether solution

出典と根拠

ORDレコード
ord-e3790a9fd059459a91df81dfebae8fa8
出典データセット
uspto-grants-1999_07
特許番号
US05929249

関連ノート

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