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

HRID 217692

반응식

HRID 217692 반응식
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][NH2:9])=[C:4]([CH3:10])[CH:3]=1.[N:11]#[C:12][Br:13]>CCO.O>[BrH:13].[Cl:1][C:2]1[CH:3]=[C:4]([CH3:10])[C:5]2[N:6]([C:12]([NH2:11])=[N:9][N:8]=2)[N:7]=1

참가 물질

5

반응물 2

HCID 10476Cyanogen BromideHCID 114464906-Chloro-3-hydrazinyl-4-methylpyridazine

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매2회

실험 절차

(6-Chloro-4-methylpyridazin-3-yl)hydrazine (W3.002; 4.6 g) were initially charged in EtOH (330 ml) and water (70 ml) while stirring at RT. Thereafter, cyanogen bromide in a mixture of EtOH (170 ml) and water (30 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 (40 g cartridge, DCM/methanol gradient of 0-10% in 30 min). 7.3 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 (40 g cartridge, DCM/methanol gradient of 0-10% in 30 min)

출처 및 근거

ORD 기록
ord-b4614576bfab4dd4b2399c21f7253d21
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198272B2

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