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

HRID 1758333노트

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HRID 1758333 반응식
[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]

참가 물질

7

반응물 5

HCID 784Hydrogen PeroxideHCID 962WaterHCID 66051Performic AcidHCID 130619371-Methyl-5-[3-(2-pyridyl)thiopropyl]thio-1,2,3,4-tetrazoleHCID 23665763Sodium Bisulfite

생성물 1

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

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

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

후처리

  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)]

출처 및 근거

ORD 기록
ord-bcd70a9f1ee143188c16d905b8f5ac1f
출처 데이터셋
uspto-grants-1983_02
특허 번호
US04372953

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