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

HRID 657909노트

반응식

HRID 657909 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매2회

실험 절차

(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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9cf55bbddfc04a248d27690ce3bc6dfc
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076336B2

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