Benzoyl chloride → 1,2,4-Triazolo(4,3-b)pyridazine, 6-(4-morpholinyl)-3-phenyl-

HRID 328068ノート

反応式

HRID 328068 の反応式
[NH:1]([C:3]1[N:4]=[N:5][C:6]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[CH:7][CH:8]=1)[NH2:2].[C:15](Cl)(=O)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(=O)(O)[O-].[Na+]>>[O:12]1[CH2:11][CH2:10][N:9]([C:6]2[CH:7]=[CH:8][C:3]3[N:4]([C:15]([C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)=[N:2][N:1]=3)[N:5]=2)[CH2:14][CH2:13]1

参加物

4

反応物 3

HCID 7412Benzoyl chlorideHCID 516892Sodium BicarbonateHCID 12603548HCID 12603548、化合物

生成物 1

HCID 15055121,2,4-Triazolo(4,3-b)pyridazine, 6-(4-morpholinyl)-3-phenyl-

実験手順

39 Grams of 3-hydrazino-6-morpholinopyridazine is added portionwise to 30 grams of benzoyl chloride. The mixture is heated at a temperature of 130°-140° C. for 1 hour. The mixture is then cooled and the residue of the reaction mixture is neutralized by the addition of aqueous sodium bicarbonate solution. The resulting aqueous mixture is then extracted with chloroform. The chloroform extract is washed with water, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The 6-morpholino-3-phenyl-s-triazolo[4,3-b]pyridazine product is obtained as a residue from the evaporation. The product is crystallized twice from isopropanol and found to melt at 195°-196° C. 15 Grams of the named product are obtained. The structure of the product is confirmed by infrared spectroscopy and by nuclear magnetic resonance analysis.

後処理

  1. temperatureThe mixture is heated at a temperature of 130°-140° C. for 1 hour
  2. temperatureThe mixture is then cooled
  3. extractionThe resulting aqueous mixture is then extracted with chloroform
  4. extractionThe chloroform extract
  5. washis washed with water
  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-df6caeb9df6144468ebdc9a80feea19f
出典データセット
uspto-grants-1977_04
特許番号
US04016162

反応ノート

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