反应详情

温度

115 °C

A Parr bomb containing 8-chloro-3-cyclobutyl-1-iodoimidazo[1,5-a]pyrazine (759 mg, 2.3 mmol) in IPA (100 mL) was saturated with NH3(g) for 5 min at 0° C. then sealed and heated at 115° C. for 38 h. The reaction mixture was then concentrated under reduced pressure, partitioned between DCM (200 mL) and H2O (50 mL) and extracted with DCM (50 mL). Combined organic fractions were washed with brine, dried (Na2SO4) and concentrated under reduced pressure to provide the title compound as a white solid; 1H NMR (400 MHz, CDCl3) δ 7.13 (d, J=4.8 Hz, 1H), 7.01 (d, J=5.2 Hz, 1H), 5.63 (br, 2H), 3.73 (quintetd, J=0.8 Hz, 8.4 Hz, 1H), 2.60-2.38 (m, 4H), 2.20-1.90 (m, 2H); MS (ES+): m/z 315.9 (100) [MH+]; HPLC: tR=1.75 min (OpenLynx, polar—5 min).

1. customthen sealed
2. concentrationThe reaction mixture was then concentrated under reduced pressure
3. custompartitioned between DCM (200 mL) and H2O (50 mL)
4. extractionextracted with DCM (50 mL)
5. washCombined organic fractions were washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated under reduced pressure