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Potassium Hydroxide → 2-Methyl-4-(3-nitrophenyl)-6-phenyl-3-pyridinecarboxylic acid

HRID 1722775
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HRID 1722775 반응식
[CH3:1][C:2]1[C:7]([C:8]([O:10]CC)=[O:9])=[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([N+:19]([O-:21])=[O:20])[CH:14]=2)[CH:5]=[C:4]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:3]=1.[OH-].[K+]>C(O)C>[CH3:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([N+:19]([O-:21])=[O:20])[CH:14]=2)[CH:5]=[C:4]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 10248079Ethyl 2-methyl-4-(3-nitrophenyl)-6-phenyl-3-pyridinecarboxylate

생성물 1

HCID 104720472-Methyl-4-(3-nitrophenyl)-6-phenyl-3-pyridinecarboxylic acid수율 46.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of ethyl 2-methyl-4-(3-nitrophenyl)-6-phenyl-3-pyridinecarboxylate (4.6 g), aqueous potassium hydroxide (1.07 g in 200 ml water) and ethanol (92 ml) was refluxed for 6 hours. After allowing to cool to ambient temperature, the reaction mixture was washed with ethyl acetate (150 ml×2). The separated aqueous layer was adjusted to pH 3.0 with 10% hydrochloric acid. To this mixture was added acetic acid (40 ml) and stirred for 30 minutes under ice cooling. The resulting precipitates were collected by filtration, washed with water and dried in vacuo to give 2-methyl-4-(3-nitrophenyl)-6-phenyl-3pyridinecarboxylic acid (1.98 g).

후처리

  1. temperaturewas refluxed for 6 hours
  2. washthe reaction mixture was washed with ethyl acetate (150 ml×2)
  3. additionTo this mixture was added acetic acid (40 ml)
  4. customThe resulting precipitates
  5. filtrationwere collected by filtration
  6. washwashed with water
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-1265deff657a4dc588613b47f926d152
출처 데이터셋
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04857527

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