Cyanogen Bromide → 6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide

HRID 657909ノート

反応式

HRID 657909 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][NH2:9])=[C:4]([CH3:10])[C:3]=1[CH3:11].[N:12]#[C:13][Br:14]>CCO.O>[BrH:14].[Cl:1][C:2]1[C:3]([CH3:11])=[C:4]([CH3:10])[C:5]2[N:6]([C:13]([NH2:12])=[N:9][N:8]=2)[N:7]=1

参加物

5

反応物 2

HCID 10476Cyanogen BromideHCID 126480423-Chloro-6-hydrazinyl-4,5-dimethylpyridazine

生成物 1

HCID 866507976-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide収率 100.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒2 回

実験手順

(6-Chloro-4,5-dimethylpyridazin-3-yl)hydrazine (W3.006; 12 g) was initially charged in EtOH (240 ml) and water (50 ml) while stirring at RT. Thereafter, cyanogen bromide (14.7 g) in a mixture of EtOH (120 ml) and water (25 ml) was slowly added dropwise at RT. After stirring at RT for 6 h, the mixture was left to stand overnight. Then the mixture was dried and the residue was purified using silica gel (80 g cartridge, DCM/methanol gradient of 0-20% in 60 min). 19.4 g of the title compound were obtained.

後処理

  1. additionwas slowly added dropwise at RT
  2. waitthe mixture was left
  3. waitto stand overnight
  4. customThen the mixture was dried
  5. customthe residue was purified
  6. customsilica gel (80 g cartridge, DCM/methanol gradient of 0-20% in 60 min)

出典と根拠

ORDレコード
ord-9cf55bbddfc04a248d27690ce3bc6dfc
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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