Piperidine → 7-Methyl-6-piperidino-s-triazolo[4,3-b]pyridazine

HRID 370444

반응식

HRID 370444 반응식
Cl[C:2]1[C:3]([CH3:11])=[CH:4][C:5]2[N:6]([CH:8]=[N:9][N:10]=2)[N:7]=1.[NH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1>C(O)C>[CH3:11][C:3]1[C:2]([N:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)=[N:7][N:6]2[CH:8]=[N:9][N:10]=[C:5]2[CH:4]=1

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 8197966-Chloro-7-methyl-[1,2,4]triazolo[4,3-b]pyridazine

생성물 1

HCID 135188117-Methyl-6-piperidino-s-triazolo[4,3-b]pyridazine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

7.8 Grams (0.0462 mole) of the 6-chloro-7-methyl-s-triazolo[4,3-b]pyridazine is mixed with 7.86 grams (0.0924 mole) of piperidine in 50 ml of ethanol. The mixture is heated at reflux temperature for 4 hours. The mixture is concentrated by evaporation and the residue of the reaction mixture is partitioned between aqueous sodium bicarbonate solution and methylene chloride. The methylene chloride layer is separated, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The 7-methyl-6-piperidino-s-triazolo[4,3-b]pyridazine product is obtained as a residue from the evaporation. The product is recrystallized from hexane and found to melt at 78°-79° C. The structure of the product is confirmed by infrared spectroscopy, by nuclear magnetic resonance analysis, and by elemental analysis. (Calculated for C11H15N5 : C, 60.80; H, 6.96; N, 32.24. Found: C, 60.40; H, 6.98; N, 32.17.)

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux temperature for 4 hours
  3. concentrationThe mixture is concentrated by evaporation
  4. customthe residue of the reaction mixture is partitioned between aqueous sodium bicarbonate solution and methylene chloride
  5. customThe methylene chloride layer is separated
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-c64ff2a37c474fefa41ee9101a711494
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04526890

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