Hydrogen Peroxide → 3-(1-Methyl-1,2,3,4-tetrazol-5-yl)sulfinylpropyl 2-pyridyl sulfoxide

HRID 1758334ノート

反応式

HRID 1758334 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7]([CH2:9][CH2:10][CH2:11][S:12][C:13]1[N:17]([CH3:18])[N:16]=[N:15][N:14]=1)=[O:8].OO.S([O-])(O)=[O:22].[Na+].C(OO)=O>C(O)=O.O>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[S:7]([CH2:9][CH2:10][CH2:11][S:12]([C:13]1[N:17]([CH3:18])[N:16]=[N:15][N:14]=1)=[O:22])=[O:8]

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 66051Performic AcidHCID 3061976Pyridine, 2-((3-((1-methyl-1H-tetrazol-5-yl)thio)propyl)sulfinyl)-HCID 23665763Sodium Bisulfite

生成物 1

HCID 130619833-(1-Methyl-1,2,3,4-tetrazol-5-yl)sulfinylpropyl 2-pyridyl sulfoxide

試薬・触媒・溶媒 2

HCID 284Formic Acid溶媒HCID 962Water溶媒

実験手順

3-(1-Methyl-1,2,3,4-tetrazol-5-yl)thiopropyl 2-pyridyl sulfoxide (2.8 g) is dissolved in formic acid (20 ml) and thereto is added with stirring 30% hydrogen peroxide (1.3 g) at room temperature, and the mixture is stirred for 5 hours. To the mixture is added sodium hydrogen sulfite under ice-cooling in order to decompose excess performic acid. Water is added to the resulting mixture and it is extracted with chloroform. The chloroform solution is washed with water and saturated aqueous sodium bicarbonate and dried over magnesium sulfate. After chloroform is distilled off, the residue is purified by column chromatography [Wakogel C-200, eluting agent, chloroform-methanol (50:1)] to give 3-(1-methyl-1,2,3,4-tetrazol-5-yl)sulfinylpropyl 2-pyridyl sulfoxide (0.8 g) as colorless liquid, nD28.5 =1.5795.

後処理

  1. additionis added
  2. temperaturecooling in order
  3. extractionis extracted with chloroform
  4. washThe chloroform solution is washed with water and saturated aqueous sodium bicarbonate
  5. dry with materialdried over magnesium sulfate
  6. distillationAfter chloroform is distilled off
  7. customthe residue is purified by column chromatography [Wakogel C-200, eluting agent, chloroform-methanol (50:1)]

出典と根拠

ORDレコード
ord-24220bbc8e6a4f76acef5842d8956398
出典データセット
uspto-grants-1983_02
特許番号
US04372953

反応ノート

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