Hydrogen Bromide → Imidazo(1,2-a)pyrazine

HRID 895116Notes

Reaction equation

HRID 895116 reaction equation
[NH2:1][C:2]1[CH:7]=[N:6][CH:5]=[CH:4][N:3]=1.CO[CH:10](OC)[CH2:11]Br.Br>C(O)C>[N:1]1[CH:10]=[CH:11][N:3]2[CH:4]=[CH:5][N:6]=[CH:7][C:2]=12

Participants

5

Procedure

2-Aminopyrazine (100 mg, 1.1 mmol) and bromoacetaldehyde dimethylacetal (253 mg, 1.6 mmol) were dissolved in ethanol (4.5 ml), hydrobromic acid (48%, 0.5 ml) added and the mixture was heated under reflux for 18 h. The solution was allowed to cool to room temperature then pre-adsorbed directly onto silica. Purification by silica gel chromatography eluting with dichloromethane and 1% conc. ammonia on a gradient of methanol (1-4%) gave imidazo[1,2-α]pyrazine (90 mg, 72%) as a white crystalline solid: δH (360 MHz, CDCl3) 6.70 (1H, s), 7.82 (1H, s), 7.88 (1H, d, J 4), 8.29 (1H, d, J 4), 9.12 (1H, s).

Workup

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 18 h
  3. customPurification by silica gel chromatography
  4. washeluting with dichloromethane and 1% conc. ammonia on a gradient of methanol (1-4%)

Sources & evidence

ORD record
ord-965bb456b74c4974b53565bd25e76edc
Source dataset
uspto-grants-2005_07
Patent number
US06914063B2

Reaction notes

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