Hydrogen Bromide → 4-(5-Methanesulfonyl-4-methyl-4H-[1,2,4]triazol-3-yl)-1H-pyridin-2-one

HRID 500547노트

반응식

HRID 500547 반응식
[CH3:1][S:2]([C:5]1[N:6]([CH3:18])[C:7]([C:10]2[CH:15]=[CH:14][N:13]=[C:12]([O:16]C)[CH:11]=2)=[N:8][N:9]=1)(=[O:4])=[O:3].Br>C(O)(=O)C.C(O)C>[CH3:1][S:2]([C:5]1[N:6]([CH3:18])[C:7]([C:10]2[CH:15]=[CH:14][NH:13][C:12](=[O:16])[CH:11]=2)=[N:8][N:9]=1)(=[O:4])=[O:3]

참가 물질

5

반응물 2

HCID 260Hydrogen BromideHCID 248518124-(5-Methanesulfonyl-4-methyl-4h-[1,2,4]triazol-3-yl)-2-methoxy-pyridine

생성물 1

HCID 248518134-(5-Methanesulfonyl-4-methyl-4H-[1,2,4]triazol-3-yl)-1H-pyridin-2-one수율 111.4%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

The title compound of example 26.1 (6.4 g, 23.9 mmol) was dissolved in acetic acid (190 mL) and 20-30% hydrogen bromide in ethanol (190 mL) was added to the reaction. It was allowed to stir at 80° C. for 3.5 hours. The reaction was concentrated once, diluted with ethanol and concentrated again. Ethanol was added once more and the mixture was sonicated until a precipitate formed. The solid was filtered and dried under vacuum to afford the title compound (6.77 g, 85%) as a white solid.

후처리

  1. concentrationThe reaction was concentrated once
  2. additiondiluted with ethanol
  3. concentrationconcentrated again
  4. additionEthanol was added once more
  5. customthe mixture was sonicated until a precipitate
  6. customformed
  7. filtrationThe solid was filtered
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-e7c2a3ea2fc44a619bf974dabd2b05a5
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772235B2

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