Sodium → Methyl 1-(3-pyridylmethyl)-2,4-dioxopiperidine-3-carboxylate

HRID 977964노트

반응식

HRID 977964 반응식
[Na].[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][N:9]([CH2:18][CH2:19][C:20]([O:22]C)=O)[C:10]([CH2:12][C:13]([O:15][CH2:16]C)=[O:14])=[O:11])[CH:3]=1>CO.C1C=CC=CC=1>[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][N:9]2[CH2:18][CH2:19][C:20](=[O:22])[CH:12]([C:13]([O:15][CH3:16])=[O:14])[C:10]2=[O:11])[CH:3]=1

참가 물질

5

반응물 2

HCID 5360545SodiumHCID 53944986Ethyl[N-(3-pyridylmethyl)-N-(methoxycarbonylethyl)carbamoyl]acetate

생성물 1

HCID 20204023Methyl 1-(3-pyridylmethyl)-2,4-dioxopiperidine-3-carboxylate수율 99.9%

시약·촉매·용매 2

HCID 241Benzene용매HCID 887Methanol용매

실험 절차

Sodium (0.77 g) is dissolved in methanol (30 ml), and thereto is added dropwise a solution of ethyl [N-(3-pyridylmethyl)-N-(methoxycarbonylethyl)carbamoyl]acetate (10.0 g) in benzene (170 ml) at 3°-8° C. The mixture is stirred at the same meperature for 2 hours. The mixture is distilled to remove the solvent, and the residue is dissolved in water. The aqueous solution is extracted with benzene, and the aqueous layer is neutralized with 10% HCl, and extracted with chloroform. The extract is dried and distilled to remove the solvent to give methyl 1-(3-pyridylmethyl)-2,4-dioxopiperidine-3-carboxylate (8.50 g, quantitative) as oil.

후처리

  1. distillationThe mixture is distilled
  2. customto remove the solvent
  3. dissolutionthe residue is dissolved in water
  4. extractionThe aqueous solution is extracted with benzene
  5. extractionextracted with chloroform
  6. customThe extract is dried
  7. distillationdistilled
  8. customto remove the solvent

출처 및 근거

ORD 기록
ord-3c8b492233f447a5b3d01e1f05db6dd9
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04663319

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