Hydrochloric Acid → 3-Cyclohexylacrylic acid

HRID 751764

反応式

HRID 751764 の反応式
[C:1](O)(=O)[CH2:2][C:3]([OH:5])=[O:4].[CH:8]1(C=O)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.Cl>N1C=CC=CC=1.N1CCCCC1>[CH:8]1([CH:1]=[CH:2][C:3]([OH:5])=[O:4])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 16275Cyclohexanecarboxaldehyde

生成物 1

HCID 2873483-Cyclohexylacrylic acid収率 107.4%

試薬・触媒・溶媒 2

HCID 8082Piperidine触媒HCID 1049Pyridine溶媒

実験手順

3.34 g (32.1 mmol) of malonic acid are dissolved in pyridine (10 ml), after the weakly exothermic reaction has subsided 3.0 g (26.7 mmol) of cyclohexanecarbaldehyde and 0.23 g (2.7 mmol) of piperidine are added, and the reaction mixture is heated to reflux for 4 h. The cooled reaction solution is added to a mixture of ice and concentrated hydrochloric acid, the aqueous phase is extracted three times with diethyl ether, the combined organic phases are dried over sodium sulfate, filtered, and the solvent is removed in vacuo. 4.42 g of product are obtained, which is reacted further without purification.

後処理

  1. customafter the weakly exothermic reaction
  2. additionare added
  3. temperaturethe reaction mixture is heated
  4. temperatureto reflux for 4 h
  5. customThe cooled reaction solution
  6. extractionthe aqueous phase is extracted three times with diethyl ether
  7. dry with materialthe combined organic phases are dried over sodium sulfate
  8. filtrationfiltered
  9. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-8ab3752884e1462380c3b22efcf07523
出典データセット
uspto-grants-2008_07
特許番号
US07405201B2

関連ノート

読み込み中…