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Potassium Iodide → N-(6-([1,2,4]triazolo[4,3-a]pyridin-3-ylthio)imidazo[1,2-b]pyridazin-2-yl)cyclopropanecarboxamide

HRID 1925104
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HRID 1925104 반응식
[N:1]1[N:2]=[C:3]([S:10][C:11]2[N:16]=[N:15][C:14]([NH2:17])=[CH:13][CH:12]=2)[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.Br[CH2:19][C:20]([NH:22][C:23]([CH:25]1[CH2:27][CH2:26]1)=[O:24])=O.P([O-])([O-])(O)=O.[K+].[K+].[I-].[K+]>CC(N(C)C)=O.CO>[N:1]1[N:2]=[C:3]([S:10][C:11]2[CH:12]=[CH:13][C:14]3[N:15]([CH:19]=[C:20]([NH:22][C:23]([CH:25]4[CH2:27][CH2:26]4)=[O:24])[N:17]=3)[N:16]=2)[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12
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참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 24450Potassium Phosphate, Dibasic2회HCID 59233013N-(2-bromoacetyl)cyclopropanecarboxamide2회HCID 592332196-([1,2,4]Triazolo[4,3-a]pyridin-3-ylthio)pyridazin-3-amine

생성물 1

HCID 46174983N-(6-([1,2,4]triazolo[4,3-a]pyridin-3-ylthio)imidazo[1,2-b]pyridazin-2-yl)cyclopropanecarboxamide수율 34.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 31374Dimethylacetamide용매

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온도
120 °C

실험 절차

A mixture of 6-([1,2,4]triazolo[4,3-a]pyridin-3-ylthio)pyridazin-3-amine (2.443 g, 10 mmol), N-(2-bromoacetyl)cyclopropanecarboxamide (3.09 g, 15.00 mmol), potassium hydrogenphosphate (5.23 g, 30.0 mmol) and potassium iodide (0.830 g, 5.00 mmol) in DMA (100 mL) was stirred at 120° C. for 2 hrs. Additional amounts of N-(2-bromoacetyl)cyclopropanecarboxamide (2.06 g, 10 mmol) and potassium hydrogenphosphate (1.74 g, 10 mmol) were added to the mixture and the reaction was stirred at 120° C. for another 2 hrs. The reaction was then stirred at room temperature overnight. The reaction mixture was again stirred at 140° C. for 3 hrs and then cooled to room temperature. The resulting solid was filtered off and rinsed with DMA. The filtrate was concentrated to 100 mL and then poured into water (300 mL). The resulting precipitate was collected by filtration and rinsed thoroughly with water. The solid material was re-suspended in 10% MeOH/CH2Cl2 (100 mL), sonicated, refluxed for 30 min and cooled to room temperature. The MeOH/CH2Cl2 solution was filtered through a silica plug, rinsed with 10% MeOH/CH2Cl2 (200 mL). To above organic solution, activated charcoal (0.5 g) was added, the solution was refluxed for 30 min, and then stirred at room temperature overnight. The charcoal was filtered through Celite, and the filtrate was concentrated to dryness to provide an off white solid. This solid was refluxed in MeOH (10 mL) for 30 min. and cooled to room temperature. The resulting off white solid was collected by filtration, rinsed with MeOH (2 mL) and dried in vacuum to provide the title compound, N-(6-([1,2,4]Triazolo[4,3-a]pyridin-3-ylthio)imidazo[1,2-b]pyridazin-2-yl)cyclopropanecarboxamide (1.2 g). 1H NMR (400 MHz, DMSO-d6) δ=11.17 (s, 1 H), 8.57-8.44 (m, 1 H), 8.03-7.94 (m, 1 H), 7.96-7.88 (m, 2 H), 7.59 (ddd, J=1.0, 6.6, 9.3 Hz, 1 H), 7.22-7.11 (m, 1 H), 7.11-7.03 (m, 1 H), 1.97-1.84 (m, 1 H), 0.83-0.73 (m, 4 H) ESI-MS:m/z 352.3 (M+H)+. MP 193-195° C.

후처리

  1. stirringthe reaction was stirred at 120° C. for another 2 hrs
  2. stirringThe reaction was then stirred at room temperature overnight
  3. stirringThe reaction mixture was again stirred at 140° C. for 3 hrs
  4. temperaturecooled to room temperature
  5. filtrationThe resulting solid was filtered off
  6. washrinsed with DMA
  7. concentrationThe filtrate was concentrated to 100 mL
  8. additionpoured into water (300 mL)
  9. filtrationThe resulting precipitate was collected by filtration
  10. washrinsed thoroughly with water
  11. customsonicated
  12. temperaturerefluxed for 30 min
  13. temperaturecooled to room temperature
  14. filtrationThe MeOH/CH2Cl2 solution was filtered through a silica plug
  15. washrinsed with 10% MeOH/CH2Cl2 (200 mL)
  16. additionwas added
  17. temperaturethe solution was refluxed for 30 min
  18. stirringstirred at room temperature overnight
  19. filtrationThe charcoal was filtered through Celite
  20. concentrationthe filtrate was concentrated to dryness
  21. customto provide an off white solid
  22. temperaturecooled to room temperature
  23. filtrationThe resulting off white solid was collected by filtration
  24. washrinsed with MeOH (2 mL)
  25. customdried in vacuum

출처 및 근거

ORD 기록
ord-aeb9d7d84dc242ca9913b7e577caca67
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178534B2

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