2-Hydroxy-4-Methoxybenzaldehyde → 3-Nicotinoyl-7-methoxycoumarin

HRID 25876

反応式

HRID 25876 の反応式
[C:1]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.O[C:16]1C=[C:22]([O:24][CH3:25])[CH:21]=[CH:20][C:17]=1C=O>N1CCCCC1>[C:1]([C:9]1[C:10](=[O:11])[O:12][C:13]2[C:17]([CH:16]=1)=[CH:20][CH:21]=[C:22]([O:24][CH3:25])[CH:14]=2)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1

参加物

4

反応物 2

HCID 696002-Hydroxy-4-MethoxybenzaldehydeHCID 222197Ethyl 3-oxo-3-(pyridin-3-yl)propanoate

生成物 1

HCID 212173313-Nicotinoyl-7-methoxycoumarin

試薬・触媒・溶媒 1

HCID 8082Piperidine触媒

実験手順

A mixture of 0.65 g ethyl nicotinoylacetate, 0.5 g 2-hydroxyanisaldehyde and 10 ml alcohol was heated on a steam bath until solution was attained. Five drops of piperdine were added and heating was continued. After several minutes the reaction mixture solidified. An additional 10 ml of alcohol were added and the reaction mixture heated another 15 minutes. After cooling, the solid was collected and recrystallized twice from a mixture of alcohol and acetonitrile.

後処理

  1. temperaturewas heated on a steam bath until solution
  2. temperatureheating
  3. waitAfter several minutes the reaction mixture solidified
  4. temperaturethe reaction mixture heated another 15 minutes
  5. temperatureAfter cooling
  6. customthe solid was collected
  7. customrecrystallized twice from a mixture of alcohol and acetonitrile

出典と根拠

ORDレコード
ord-0df72b8e35584857b395332273362433
出典データセット
uspto-grants-1979_04
特許番号
US04147552

関連ノート

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