Ethanol → HCID 178418414, 화합물

HRID 2344

반응식

HRID 2344 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 178418414HCID 178418414, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2843bd13368f422ab3826093b175bc25
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728842

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