Sodium Sulfite → 3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-sulfopyridine

HRID 37510

반응식

HRID 37510 반응식
[S:1]([O-:4])([O-:3])=[O:2].[Na+].[Na+].Cl[C:8]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[C:11]([N+:24]([O-:26])=[O:25])=[C:10]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[N:9]=1>O.C(O)C>[CH2:17]([O:16][C:14]([C:13]1[C:8]([S:1]([OH:4])(=[O:3])=[O:2])=[N:9][C:10]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[C:11]([N+:24]([O-:26])=[O:25])[C:12]=1[C:19]([O:21][CH2:22][CH3:23])=[O:20])=[O:15])[CH3:18]

참가 물질

5

반응물 2

HCID 24437Sodium SulfiteHCID 199355872-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine

생성물 1

HCID 199356093,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-sulfopyridine수율 59.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 0.28 g of sodium sulfite in 7 ml of water was added to a solution of 0.70 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine in 7 ml of ethanol, and the mixture was heated under reflux for minutes. After the reaction mixture was concentrated, the concentrate was acidified with 1N HCl, followed by extraction with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over magnesium sulfate. After concentration to dryness under reduced pressure, the residue was recrystallized from chloroform/ether, to give 0.47 g of white crystals.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for minutes
  3. concentrationAfter the reaction mixture was concentrated
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. concentrationAfter concentration to dryness under reduced pressure
  8. customthe residue was recrystallized from chloroform/ether

출처 및 근거

ORD 기록
ord-b90069235e134fd59f7501c27c3f1a71
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420275

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