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Methyl Isobutyl Ketone → 5-Ethylquinolinic acid

HRID 1654997
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HRID 1654997 반응식
[CH2:1]([C:3]1[CH:4]=[C:5]([C:12]([OH:14])=[O:13])[C:6]([C:9]([OH:11])=[O:10])=[N:7][CH:8]=1)[CH3:2].[CH2:15](C(C)=O)[CH:16](C)C>C(Cl)Cl>[CH2:1]([C:3]1[CH:4]=[C:5]([C:12]([OH:14])=[O:13])[C:6]([C:9]([OH:11])=[O:10])=[N:7][CH:8]=1)[CH3:2].[CH2:1]([C:3]1[CH:8]=[N:7][C:6]2[C:5]([CH:4]=1)=[CH:12][CH:16]=[CH:15][C:9]=2[OH:11])[CH3:2]
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참가 물질

5

반응물 2

HCID 7909Methyl Isobutyl KetoneHCID 1136065-Ethylquinolinic acid

생성물 2

HCID 1136065-Ethylquinolinic acidHCID 117896928-Quinolinol, 3-ethyl-

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Preparation of 5-ethyl-2,3-pyridinedicarboxylic acid ##STR6## The nitrate salt obtained in Example 1 is dispersed in a mixture of 100 mL of methylene chloride and 100 mL of methyl isobutyl ketone, heated at reflux temperature for 1 hour, cooled to room temperature and filtered. The filter cake is washed with a 1:1 mixture of methylene chloride:methyl isobutyl ketone and dried in vacuo to give 5-ethyl-2,3-pyridinedicarboxylic acid, 34.6 g, (89% isolated yield from 3-ethyl-8-hydroxyquinoline), 94.5% pure by HPLC.

후처리

  1. temperatureheated
  2. temperatureat reflux temperature for 1 hour
  3. filtrationfiltered
  4. washThe filter cake is washed with a 1:1 mixture of methylene chloride
  5. dry with materialmethyl isobutyl ketone and dried in vacuo
  6. customto give

출처 및 근거

ORD 기록
ord-481e833f983f43439f019f5f82b4155c
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05410062

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