Water → Pyridine, 2-[[(2,5-dimethylphenyl)methyl]sulfonyl]-3-methyl-, 1-oxide

HRID 1829735노트

반응식

HRID 1829735 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][N+:12]=1[O-:18].[OH:19]OS([O-])=O.[K+].[OH2:25]>CO>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[CH2:9][S:10]([C:11]1[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][N+:12]=1[O-:18])(=[O:19])=[O:25]

참가 물질

5

반응물 3

HCID 962Water2회HCID 131787402-{[(2,5-Dimethylphenyl)methyl]sulfanyl}-3-methyl-1-oxo-1lambda~5~-pyridineHCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 9900653Pyridine, 2-[[(2,5-dimethylphenyl)methyl]sulfonyl]-3-methyl-, 1-oxide

시약·촉매·용매 1

HCID 887Methanol용매

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온도
24 °C

실험 절차

To a stirred solution of 4.0 g of 2-[((2,5-dimethylphenyl)methyl)thio]-3-methylpyridine-1-oxide in 50 mL of methanol, cooled to 3° C., was added a solution of 14.1 g of Oxone® in 50 mL of water over a period of 50 minutes. The reaction mixture was stirred at 24° C. overnight and then diluted with 200 mL of water. The product was extracted into chloroform and dried over magnesium sulfate. Evaporation of solvent under reduced pressure gave 4.1 g of 2-[((2,5-dimethylphenyl)methyl)sulfonyl]-3-methylpyridine-1-oxide as a white crystalline solid, having a melting point of 171–173° C. The 1H NMR spectrum (CDCl3) was in agreement with the expected structure.

후처리

  1. extractionThe product was extracted into chloroform
  2. dry with materialdried over magnesium sulfate
  3. customEvaporation of solvent under reduced pressure

출처 및 근거

ORD 기록
ord-d95b33a64a194054a549499545d5d6ea
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064139B2

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