Dimethylformamide → N6,n6-diethyl-8-methyl-1,2,4-triazolo[4,3-b]pyridazine-3,6-diamine

HRID 532328

反応式

HRID 532328 の反応式
Br.Cl[C:3]1[CH:4]=[C:5]([CH3:13])[C:6]2[N:7]([C:9]([NH2:12])=[N:10][N:11]=2)[N:8]=1.CN(C=O)C.[CH2:19]([NH:21][CH2:22][CH3:23])[CH3:20]>O>[CH2:19]([N:21]([CH2:22][CH3:23])[C:3]1[CH:4]=[C:5]([CH3:13])[C:6]2[N:7]([C:9]([NH2:12])=[N:10][N:11]=2)[N:8]=1)[CH3:20]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 8021DiethylamineHCID 866507966-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide

生成物 1

HCID 58136920N6,n6-diethyl-8-methyl-1,2,4-triazolo[4,3-b]pyridazine-3,6-diamine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

6-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.002; 250 mg) was dissolved in abs. DMF (2 ml) and admixed with diethylamine (7 ml). Thereafter, the reaction mixture was placed into a heating block at 80° C. with stirring for 11 days. The solvent was then drawn off and the residue was admixed with a little water and extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue was purified by means of preparative HPLC (met. A), and the clean product fractions were combined, freed of the acetonitrile under reduced pressure, alkalized with saturated potassium carbonate solution and extracted repeatedly with dichloromethane. The combined organic phases were dried over sodium sulfate, filtered and concentrated. 100 mg of the title compound were obtained.

後処理

  1. customwas placed into a heating block at 80° C.
  2. extractionextracted three times with dichloromethane
  3. dry with materialThe combined organic phases were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by means of preparative HPLC (
  7. extractionextracted repeatedly with dichloromethane
  8. dry with materialThe combined organic phases were dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-57fe8b7eebf643ec8c8f3dfe134f3fc0
出典データセット
uspto-grants-2014_10
特許番号
US08853206B2

関連ノート

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