Diethylamine → N*6*,N*6*-Diethyl-[1,2,4]triazolo[4,3-b]pyridazine-3,6-diamine

HRID 657854ノート

反応式

HRID 657854 の反応式
Br.Cl[C:3]1[CH:4]=[CH:5][C:6]2[N:7]([C:9]([NH2:12])=[N:10][N:11]=2)[N:8]=1.[CH2:13]([NH:15][CH2:16][CH3:17])[CH3:14]>O>[CH2:13]([N:15]([CH2:16][CH3:17])[C:3]1[CH:4]=[CH:5][C:6]2[N:7]([C:9]([NH2:12])=[N:10][N:11]=2)[N:8]=1)[CH3:14]

参加物

4

反応物 2

HCID 8021Diethylamine2 回HCID 866507946-Chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide

生成物 1

HCID 58136803N*6*,N*6*-Diethyl-[1,2,4]triazolo[4,3-b]pyridazine-3,6-diamine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

6-Chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.001; 150 mg) was initially charged in water (5 ml) and admixed with diethylamine (814 μl) while stirring. Thereafter, the mixture was heated to reflux for 16 h and then further diethylamine (407 μl) was added. After refluxing for a further 12 h, the mixture was freed of the solvent, admixed with water and extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. 67 mg of the title compound were obtained.

後処理

  1. temperatureThereafter, the mixture was heated
  2. temperatureto reflux for 16 h
  3. temperatureAfter refluxing for a further 12 h
  4. extractionextracted three times with dichloromethane
  5. dry with materialThe combined organic phases were dried over sodium sulfate
  6. filtrationafter the desiccant had been filtered off
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-767e0679d28446d29bb1363943d52ae6
出典データセット
uspto-grants-2011_12
特許番号
US08076336B2

反応ノート

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