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

HRID 1758333ノート

反応式

HRID 1758333 の反応式
[CH3:1][N:2]1[C:6]([S:7][CH2:8][CH2:9][CH2:10][S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)=[N:5][N:4]=[N:3]1.OO.S([O-])(O)=[O:21].[Na+].C(OO)=O.[OH2:29]>C(O)=O>[N:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[S:11]([CH2:10][CH2:9][CH2:8][S:7]([C:6]1[N:2]([CH3:1])[N:3]=[N:4][N:5]=1)=[O:21])=[O:29]

参加物

7

反応物 5

HCID 784Hydrogen PeroxideHCID 962WaterHCID 66051Performic AcidHCID 13061937HCID 13061937、化合物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 1

HCID 284Formic Acid溶媒

実験手順

1-Methyl-5-[3-(2-pyridyl)thiopropyl]thio-1,2,3,4-tetrazole (2.2 g) is dissolved in formic acid (20 ml), and thereto is added with stirring 30% hydrogen peroxide (2.2 g) at room temperature. The mixture is stirred at room temperature for 5 hours, and thereto is added sodium hydrogensulfite under ice-cooling in order to decompose excess amount of performic acid. Water is added to the mixture and the mixture 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 [Kieselgel 60, eluting agent, chloroform-methanol (50:1)] to give 3-(1-methyl-1,2,3,4-tetrazol-5-yl)sulfinylpropyl 2-pyridyl sulfoxide (0.5 g) as colorless liquid, nD28.5 =1.5795

後処理

  1. additionis added
  2. temperaturecooling in order
  3. extractionthe mixture is 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 [Kieselgel 60, eluting agent, chloroform-methanol (50:1)]

出典と根拠

ORDレコード
ord-bcd70a9f1ee143188c16d905b8f5ac1f
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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