反应详情

温度

100 °C

The title compound was prepared following the procedure described in Example 62, with the deprotection of the purine performed as follows. A glass microwave reaction vessel was charged with 5-chloro-N-(6-methoxypyridin-3-yl)-3-(2-methyl-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-yl)pyridin-2-amine (0.100 g, 0.221 mmol) and 1.0 M hydrochloric acid (1.106 mL, 1.106 mmol) in THF (2 ml). The reaction mixture was stirred and heated in a Discover model microwave reactor (CEM, Matthews, N.C.) at 100° C. for 10 minutes (100 watts, Powermax feature on). The mixture was diluted with DCM, made basic (pH about 12) with 1 N NaOH and allowed mixture to stir for 10 min. The precipitate was collected by filtration and washed with diethyl ether to give 5-chloro-N-(6-methoxypyridin-3-yl)-3-(2-methyl-9H-purin-6-yl)pyridin-2-amine (0.060 g, 0.163 mmol, 73.7% yield) as a yellow solid. 1H NMR (400 MHz, d6-DMSO) δ 13.83 (s, 1H); 10.24 (s, 1H); 8.54 (s, 1H); 8.18 (s, 2H); 8.06 (s, 1H); 3.85 (s, 3H); 2.73 (s, 3H); 1.62 (s, 2H). m/z (ESI, +ve ion) 367.9 (M+H)+.

1. customThe title compound was prepared
2. customA glass microwave reaction vessel
3. stirringto stir for 10 min
4. filtrationThe precipitate was collected by filtration
5. washwashed with diethyl ether