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

HRID 1829735ノート

反応式

HRID 1829735 の反応式
[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]

参加物

5

反応物 3

HCID 962Water2 回HCID 131787402-{[(2,5-Dimethylphenyl)methyl]sulfanyl}-3-methyl-1-oxo-1lambda~5~-pyridineHCID 23707502Potassium hydroxy sulfite

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
24 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d95b33a64a194054a549499545d5d6ea
出典データセット
uspto-grants-2006_06
特許番号
US07064139B2

反応ノート

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