Hydrochloric Acid → 3-Cyclohexylacrylic acid

HRID 751764

반응식

HRID 751764 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 16275Cyclohexanecarboxaldehyde

생성물 1

HCID 2873483-Cyclohexylacrylic acid수율 107.4%

시약·촉매·용매 2

HCID 8082Piperidine촉매HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8ab3752884e1462380c3b22efcf07523
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405201B2

연결된 노트

불러오는 중…