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

HRID 37510

反応式

HRID 37510 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b90069235e134fd59f7501c27c3f1a71
出典データセット
uspto-grants-1995_05
特許番号
US05420275

関連ノート

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