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

HRID 370444

反応式

HRID 370444 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.)

後処理

  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

出典と根拠

ORDレコード
ord-c64ff2a37c474fefa41ee9101a711494
出典データセット
uspto-grants-1985_07
特許番号
US04526890

関連ノート

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