Formic Acid → 1,2,4-Triazolo(4,3-b)pyridazine, 8-methyl-6-(4-morpholinyl)-

HRID 2163660ノート

反応式

HRID 2163660 の反応式
[NH:1]([C:3]1[N:4]=[N:5][C:6]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)=[CH:7][C:8]=1[CH3:9])[NH2:2].[CH:16](O)=O>>[CH3:9][C:8]1[C:3]2[N:4]([CH:16]=[N:2][N:1]=2)[N:5]=[C:6]([N:10]2[CH2:11][CH2:12][O:13][CH2:14][CH2:15]2)[CH:7]=1

参加物

3

反応物 2

HCID 284Formic AcidHCID 216109Morpholine, 4-(6-hydrazino-5-methyl-2-pyridazinyl)-, dihydrochloride, hydrate

生成物 1

HCID 30439401,2,4-Triazolo(4,3-b)pyridazine, 8-methyl-6-(4-morpholinyl)-

実験手順

20 Grams of 3-hydrazino-4-methyl-6morpholinopyridazine are dispersed in 200 milliliters of 99 percent aqueous formic acid. The mixture is heated at the boiling temperature under reflux and then concentrated until an oily residue remains in the reaction vessel. The residue is taken up in aqueous sodium carbonate solution, and the aqueous mixture is extracted with chloroform. The chloroform extract is dried with anhydrous sodium sulfate, then evaporated under reduced pressure to obtain the 8-methyl-6-morpholino-s-triazolo[4,3-b]pyridazine product as the free base. The product is recrystallized twice from isopropanol and found to melt at 177°-178° C.

後処理

  1. temperatureThe mixture is heated at the boiling temperature
  2. temperatureunder reflux
  3. concentrationconcentrated until an oily residue
  4. extractionthe aqueous mixture is extracted with chloroform
  5. extractionThe chloroform extract
  6. dry with materialis dried with anhydrous sodium sulfate
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-6ef2cad846db40e496f93ecdc079dd81
出典データセット
uspto-grants-1979_01
特許番号
US04136182

反応ノート

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