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2-Chloroaniline → HCID 13002203, 화합물

HRID 461670
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HRID 461670 반응식
[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].[CH3:9][C:10]1([CH3:18])[CH2:17][C:15](=O)[CH2:14][C:12](=[O:13])[CH2:11]1>C(O)C.C(O)(=O)C>[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH:4][C:15]1[CH2:17][C:10]([CH3:18])([CH3:9])[CH2:11][C:12](=[O:13])[CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 72402-ChloroanilineHCID 31358Dimedone

생성물 1

HCID 13002203HCID 13002203, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid촉매HCID 702Ethanol용매

실험 절차

A mixture of 12.75 parts of 2-chloroaniline and 14 parts of dimedone is dissolved in 40 volume parts of ethanol under warming, followed by the addition of 3 drops of glacial acetic acid. The solution is refluxed in a water bath for 2 hours, after which time the ethanol is distilled off and the resulting residue is allowed to cool, whereupon yellow crystals separate. These crystals are collected by filtration, washed with isopropyl ether and recrystallized from acetone. The procedure yields 3-(2-chloroanilino)-5,5-dimethyl-2-cyclohexen-1-one as colorless prisms melting at 150°-152° C.

후처리

  1. temperatureunder warming
  2. temperatureThe solution is refluxed in a water bath for 2 hours
  3. distillationafter which time the ethanol is distilled off
  4. temperatureto cool
  5. customwhereupon yellow crystals separate
  6. filtrationThese crystals are collected by filtration
  7. washwashed with isopropyl ether
  8. customrecrystallized from acetone

출처 및 근거

ORD 기록
ord-6c8f98a6b9d14018a65478f83f65df90
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04064133

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