Diethyl Malonate → HCID 18784169、化合物

HRID 1108753ノート

反応式

HRID 1108753 の反応式
[C:1]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:2][C:3]([O:5]CC)=O.CC(C)([O-])C.[K+].[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH:28]=[CH:29][C:30](=[O:32])[CH3:31])[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]>C(O)C>[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH:28]2[CH2:29][C:30](=[O:32])[CH2:31][C:3](=[O:5])[CH:2]2[C:1]([O:9][CH2:10][CH3:11])=[O:8])[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]

参加物

5

反応物 3

HCID 7761Diethyl MalonateHCID 847484-(3,4-Dimethoxyphenyl)but-3-en-2-oneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 18784169HCID 18784169、化合物収率 871.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Diethyl malonate (73. 7 g) was dissolved in ethanol (700 ml), and then potassium tert-butoxide (51.6 g) was gradually added thereto. A solution of 4-(3,4-dimethoxyphenyl)-3-buten-2-one (79.1 g) in ethanol (500 ml) was added dropwise, and the mixture was refluxed for 1.5 hours. After distilling off the reaction solvent under reduced pressure, ice water was poured over it and it was adjusted to pH4 with concentrated hydrochloric acid. The deposited crystals were filtered by suction, washed with water and then air-dried to give 122 g of ethyl 2-(3,4-dimethoxyphenyl)-4,6-dioxocyclohexane carboxylate (99.6%).

後処理

  1. temperaturethe mixture was refluxed for 1.5 hours
  2. distillationAfter distilling off the reaction solvent under reduced pressure, ice water
  3. additionwas poured over it and it
  4. filtrationThe deposited crystals were filtered by suction
  5. washwashed with water
  6. customair-dried

出典と根拠

ORDレコード
ord-9c21202cffce45829b9f67d9e3bde488
出典データセット
uspto-grants-2000_05
特許番号
US06069176

反応ノート

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