4-Ethoxybenzaldehyde → 3-(4-Ethoxycinnamoyl)-7-methoxycoumarin

HRID 25874

反応式

HRID 25874 の反応式
[C:1]([C:4]1[C:5](=[O:16])[O:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[C:9]([O:14][CH3:15])[CH:8]=2)(=[O:3])[CH3:2].[CH2:17]([O:19][C:20]1[CH:27]=[CH:26][C:23]([CH:24]=O)=[CH:22][CH:21]=1)[CH3:18]>N1CCCCC1.C(#N)C>[CH2:17]([O:19][C:20]1[CH:27]=[CH:26][C:23]([CH:24]=[CH:2][C:1]([C:4]2[C:5](=[O:16])[O:6][C:7]3[C:12]([CH:13]=2)=[CH:11][CH:10]=[C:9]([O:14][CH3:15])[CH:8]=3)=[O:3])=[CH:22][CH:21]=1)[CH3:18]

参加物

5

反応物 2

HCID 248344-EthoxybenzaldehydeHCID 20544753-Acetyl-7-methoxycoumarin

生成物 1

HCID 541146183-(4-Ethoxycinnamoyl)-7-methoxycoumarin

試薬・触媒・溶媒 2

HCID 8082Piperidine触媒2 回HCID 6342Acetonitrile溶媒

実験手順

A suspension of 2.18 g 3-acetyl-7-methoxycoumarin and 1.65 g p-ethoxybenzaldehyde in 100 ml alcohol was heated under reflux on a steam bath. Acetonitrile was added until solution was attained. Fifty drops of piperidine were added and the reaction mixture heated under reflux for 90 minutes. An additional fifty drops of piperidine were added and the solution was heated under reflux another hour. The product separated upon cooling and was washed with alcohol before being recrystallized from a mixture of alcohol and acetonitrile.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux on a steam bath
  3. temperaturethe reaction mixture heated
  4. temperatureunder reflux for 90 minutes
  5. temperaturethe solution was heated
  6. temperatureunder reflux another hour
  7. customThe product separated
  8. temperatureupon cooling
  9. washwas washed with alcohol
  10. custombefore being recrystallized from a mixture of alcohol and acetonitrile

出典と根拠

ORDレコード
ord-943fff4c598841fc8e0531cb49187a38
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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