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

HRID 500546노트

반응식

HRID 500546 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d4a2b11b39e84215a1fcec443b3fdc39
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772235B2

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