Methanol → 4-(5-Methanesulfonyl-4-methyl-4h-[1,2,4]triazol-3-yl)-2-methoxy-pyridine

HRID 500546ノート

反応式

HRID 500546 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[N:13]([CH3:14])[C:12](SC)=[N:11][N:10]=2)[CH:6]=[CH:5][N:4]=1.O[O:18][S:19]([O-:21])=O.[K+].S([O-])(O[O-])(=O)=O.[K+].[K+].[CH3:31]O>O>[CH3:31][S:19]([C:12]1[N:13]([CH3:14])[C:9]([C:7]2[CH:6]=[CH:5][N:4]=[C:3]([O:2][CH3:1])[CH:8]=2)=[N:10][N:11]=1)(=[O:21])=[O:18]

参加物

6

反応物 4

HCID 887MethanolHCID 10313463Potassium peroxymonosulphateHCID 23707502Potassium hydroxy sulfiteHCID 248517082-Methoxy-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-pyridine

生成物 1

HCID 248518124-(5-Methanesulfonyl-4-methyl-4h-[1,2,4]triazol-3-yl)-2-methoxy-pyridine収率 93%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The title compound of example 25.1 (21.97 g, 92.97 mmol) was partially dissolved in methanol (500 mL) and OXONE® (potassium peroxomonosulfate compound, 114.3 g, 186.0 mmol) dissolved in water (500 mL) was added slowly. The reaction mixture stirred for 5 hours. The reaction was partially concentrated, poured into water and extracted with chloroform. The organic extracts were dried, filtered and concentrated to afford the title compound (22 g, 93%) as a white solid.

後処理

  1. additionwas added slowly
  2. concentrationThe reaction was partially concentrated
  3. additionpoured into water
  4. extractionextracted with chloroform
  5. customThe organic extracts were dried
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-d4a2b11b39e84215a1fcec443b3fdc39
出典データセット
uspto-grants-2010_08
特許番号
US07772235B2

反応ノート

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