反应详情

温度

80 °C

A mixture of 4-chloro-1H-pyrazolo[3,4-d]pyrimidin-6-ylamine (158 mg), crude 4-chloro-2-chloromethyl-3,5-dimethyl-pyridine (204 mg), Cs2CO3 (660 mg) and DMF was heated to 80° C. for 1.5 h, diluted with EtOAc and washed with water. The crude material was concentrated and suspended in MeOH/DCM. Filtration gave a 2:1 mixture of regioisomers which was further purified by preparative silica gel plate (EtOAc 100%). The major (less polar) isomer corresponded to the title compound. R.t. 5.45 min. 1H-NMR (CDCl3) δ 8.22 (s, 1H), 7.90 (s, 1H), 5.57 (s, 2H), 5.28 (s, 2H), 2.43 (s, 3H), 2.31 (s, 3H).

1. washwashed with water
2. concentrationThe crude material was concentrated
3. filtrationFiltration
4. customgave
5. additiona 2:1 mixture of regioisomers which
6. customwas further purified by preparative silica gel plate (EtOAc 100%)
7. custom5.45 min