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Methane → HCID 20232094, 화합물

HRID 2290360
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HRID 2290360 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[N:13][NH:14][C:15]([NH2:17])=[S:16])[C:9](=NO)[CH3:10])=[CH:4][CH:3]=1.[C:18](=O)([O-])[O-].[K+].[K+].C>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:13]=[N:14][C:15]([S:16][CH3:18])=[N:17][C:9]=2[CH3:10])=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 297MethaneHCID 11430Potassium CarbonateHCID 136332165HCID 136332165, 화합물

생성물 1

HCID 20232094HCID 20232094, 화합물수율 58%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 4'-chloro-2-hydroxyiminopropiophenone thiosemicarbazone (113.21 g), potassium carbonate (128.71 g) and water (990 ml) was refluxed for 25 hours with stirring, and the reaction mixture was treated with activated charcoal and filtered by suction. To the filtrate was added dropwise methyl iodide (76 g) with stirring, and the stirring was continued for 15 minutes at room temperature. The resulting solid was collected by filtration, washed with water and dissolved in chloroform. The solution was treated with silica gel and filtered, and the filtrate was evaporated under reduced pressure. The residue was washed with diisopropyl ether and dried to give a solid of 6-(4-chlorophenyl)-5-methyl-3-methylthio-1,2,4-triazine (61.1 g).

후처리

  1. temperaturewas refluxed for 25 hours
  2. filtrationfiltered by suction
  3. additionTo the filtrate was added dropwise methyl iodide (76 g)
  4. stirringwith stirring
  5. filtrationThe resulting solid was collected by filtration
  6. washwashed with water
  7. dissolutiondissolved in chloroform
  8. additionThe solution was treated with silica gel
  9. filtrationfiltered
  10. customthe filtrate was evaporated under reduced pressure
  11. washThe residue was washed with diisopropyl ether
  12. customdried

출처 및 근거

ORD 기록
ord-44c74fc1e3dd4da9b4bab78e05011164
출처 데이터셋
uspto-grants-1986_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04616014

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