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

HRID 977964ノート

反応式

HRID 977964 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3c8b492233f447a5b3d01e1f05db6dd9
出典データセット
uspto-grants-1987_05
特許番号
US04663319

反応ノート

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