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Chloroform → 3-(4-Methyl-5-(methylsulfonyl)-4H-1,2,4-triazol-3-yl)pyridine

HRID 639832
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HRID 639832 반응식
[O-:1][Mn](=O)(=O)=O.[K+].[CH3:7][N:8]1[C:12]([S:13][CH3:14])=[N:11][N:10]=[C:9]1[C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1.[OH-:21].[Na+].C(Cl)(Cl)Cl>O.C(O)(=O)C>[CH3:7][N:8]1[C:12]([S:13]([CH3:14])(=[O:1])=[O:21])=[N:11][N:10]=[C:9]1[C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6212ChloroformHCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 404246263-(4-Methyl-5-(methylthio)-4H-1,2,4-triazol-3-yl)pyridine

생성물 1

HCID 469283343-(4-Methyl-5-(methylsulfonyl)-4H-1,2,4-triazol-3-yl)pyridine수율 53%

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 962Water용매

실험 절차

KMnO4 (5 g, 32 mmol) was added to a solution of 3-[4-methyl-5-(methylthio)-4H-1,2,4-triazol-3-yl]pyridine (6.0 g, 29 mmol) in H2O (40 mL) and acetic acid (100 mL). After 1 h stirring at r.t. the reaction was basified with 4M NaOH. CHCl3 was added and the mixture was filtrated through celite. The layers were separated and the water phase was washed with CHCl3. The combined organic phase was dried and concentrated to give 3.67 g (53%) of the title compound. 1H NMR: 3.59 (s, 3H) 3.99 (s, 3H) 7.52 (m, 1H) 8.02 (dt, 1H) 8.83 (dd, 1H) 8.91 (m, 1H)

후처리

  1. filtrationthe mixture was filtrated through celite
  2. customThe layers were separated
  3. washthe water phase was washed with CHCl3
  4. customThe combined organic phase was dried
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1c56794da5e74e969e17e292ac3b107b
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691892B2

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