反应详情

温度

170 °C

50 mg (0.09 mmol) of 2-[1-(2-fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazol-3-yl]-4-iodo-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one (example 33A) was dissolved in 1 ml of absolute NMP and 336 mg (3.70 mmol) of 2,2,2-trifluoroethanamine was added. The mixture was heated in the microwave for 2 h at 150° C., 18 h at 150° C., 2 h at 160° C., 2 h at 170° C. and 5 h at 170° C. The reaction solution was filtered and purified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→100:0). 18 mg (purity 88%, 36% of theor.) of the target compound was obtained.

1. filtrationThe reaction solution was filtered
2. custompurified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→100:0)
3. custom18 mg (purity 88%, 36% of theor.) of the target compound was obtained