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Methyl iodide → 4-(4-Methyl-5-(methylthio)-4H-1,2,4-triazol-3-yl)pyridine

HRID 703127
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HRID 703127 반응식
[CH3:1][N:2]1[C:6]([C:7]2[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=2)=[N:5][NH:4][C:3]1=[S:13].[C:14]([O-])([O-])=O.[K+].[K+].CI>CC(C)=O>[CH3:1][N:2]1[C:3]([S:13][CH3:14])=[N:4][N:5]=[C:6]1[C:7]1[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 7385474-methyl-5-(pyridin-4-yl)-4H-1,2,4-triazole-3-thiol

생성물 1

HCID 8659874-(4-Methyl-5-(methylthio)-4H-1,2,4-triazol-3-yl)pyridine

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 2,4-dihydro-4-methy-5-(4-pyridyl)-3H-1,2,4-triazole-3-thione (4.19 g, 2.18×10-2 mole), K2CO3 (3.01 g, 2.18×10-2 mole), methyl iodide (1.5 ml, 2.4×10-2 mole), and acetone (65 ml) was stirred and warmed to reflux. After refluxing overnight, the solvent was evaporated at reduced pressure and the concentrate was treated with water. The aqueous mixture was extracted with EtOAc three times. The EtOAc extracts were combined, washed with saturated aqueous NaCl, and dried over anhydrous Na2SO4. The drying agent was removed by filtration and the filtrate was evaporated at reduced pressure to yield the desired product.

후처리

  1. temperaturewarmed to reflux
  2. temperatureAfter refluxing overnight
  3. customthe solvent was evaporated at reduced pressure
  4. additionthe concentrate was treated with water
  5. extractionThe aqueous mixture was extracted with EtOAc three times
  6. washwashed with saturated aqueous NaCl
  7. dry with materialdried over anhydrous Na2SO4
  8. customThe drying agent was removed by filtration
  9. customthe filtrate was evaporated at reduced pressure

출처 및 근거

ORD 기록
ord-b5771cf1c9994dbc8100d98152a61905
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04981863

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