Ethyl cyanoacetate → Ethyl 4-acetamido-alpha-cyanocinnamate

HRID 133688

反応式

HRID 133688 の反応式
[C:1]([CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])#[N:2].[C:9]([NH:12][C:13]1[CH:20]=[CH:19][C:16]([CH:17]=O)=[CH:15][CH:14]=1)(=[O:11])[CH3:10].N1CCCCC1>C(O)C>[C:9]([NH:12][C:13]1[CH:20]=[CH:19][C:16]([CH:17]=[C:3]([C:1]#[N:2])[C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH:15][CH:14]=1)(=[O:11])[CH3:10]

参加物

5

反応物 3

HCID 7764Ethyl cyanoacetateHCID 8082PiperidineHCID 739424-Acetamidobenzaldehyde

生成物 1

HCID 245851Ethyl 4-acetamido-alpha-cyanocinnamate収率 41.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A mixture of 33.9 g (0.3 mol) of ethyl cyanoacetate and 59.1 g (0.3 mol) of 4-acetamidobenzaldehyde in 300 ml of ethanol in the presence of 5 ml of piperidine is refluxed for 3 hours. The very viscous medium is diluted with 800 ml of hot ethanol. It is filtered while hot. The yellow solid obtained is washed with hot ethanol. After filtration and drying, 32 g (41% yield) of ethyl 3-(4-acetylaminophenyl)-2-cyanoacrylate are obtained in the form of a pale yellow powder.

後処理

  1. temperatureis refluxed for 3 hours
  2. filtrationIt is filtered while hot
  3. customThe yellow solid obtained
  4. washis washed with hot ethanol
  5. filtrationAfter filtration
  6. customdrying

出典と根拠

ORDレコード
ord-0de7e36560a4413c9a7044cf947d16d7
出典データセット
uspto-grants-2008_06
特許番号
US07390916B2

関連ノート

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