1-Piperazinecarboxylic acid, ethyl ester → HCID 13957253、化合物

HRID 2308948ノート

反応式

HRID 2308948 の反応式
[N:1]1[C:10]2[C:9](=[O:11])[CH:8]=[CH:7][C:6](=[O:12])[C:5]=2[CH:4]=[CH:3][CH:2]=1.[N:13]1([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>COCCOC.[Ag]=O>[CH2:22]([O:21][C:19]([N:13]1[CH2:14][CH2:15][N:16]([C:7]2[C:6](=[O:12])[C:5]3[CH:4]=[CH:3][CH:2]=[N:1][C:10]=3[C:9](=[O:11])[CH:8]=2)[CH2:17][CH2:18]1)=[O:20])[CH3:23]

参加物

5

反応物 2

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 3883065,8-Dihydroquinoline-5,8-dione

生成物 1

HCID 13957253HCID 13957253、化合物収率 37.5%

試薬・触媒・溶媒 2

HCID 92152Silver(II) oxide触媒HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

A mixture of 1.1 g of 5,8-quinolinedione in 100 ml of 1,2-dimethoxyethane was added dropwise to a solution of 2.37 g of 1-piperazinecarboxylic acid, ethyl ester in 25 ml of 1,2-dimethyoxyethane with stirring. Stirring was continued for 30 minutes, then 1 g of silver oxide was added and this mixture was stirred overnight. The mixture was filtered and the solid washed with dichloromethane. The filtrate and wash were combined, evaporated, triturated with ethyl acetate and the solid collected. This solid was chromatographed, eluting with dichloromethane, then ethyl acetate. The active fractions were combined and evaporated, giving 817 mg of the desired product, mp 192°-194° C. (dec.).

後処理

  1. stirringStirring
  2. stirringthis mixture was stirred overnight
  3. filtrationThe mixture was filtered
  4. washthe solid washed with dichloromethane
  5. washThe filtrate and wash
  6. customevaporated
  7. customtriturated with ethyl acetate
  8. customthe solid collected
  9. customThis solid was chromatographed
  10. washeluting with dichloromethane
  11. customevaporated

出典と根拠

ORDレコード
ord-095caf2d3c304d4faf785367e1c7d6dc
出典データセット
uspto-grants-1987_09
特許番号
US04692449

反応ノート

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