反应详情

温度

60 °C

Thieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidine-9-carbonitrile (251 mg, 1.25 mmol) was dissolved in MeOH (6.2 mL), and N1-methylethane-1,2-diamine (0.22 mL, 2.5 mmol) was added. This was heated to 60° C. for 20 min, then immediately cooled in an ice bath. Saturated NH4Cl (30 mL) was added, then the aqueous mixture was extracted with 10% iPrOH/CHCl3 (3×). The organic layers were combined, dried (MgSO4), filtered and concentrated under reduced pressure to give the titled compound as a single peak on LC/MS: method [4], retention time=0.658 min; MS (ESI) 192.0 (MH+).

1. temperatureimmediately cooled in an ice bath
2. extractionthe aqueous mixture was extracted with 10% iPrOH/CHCl3 (3×)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure