反应详情

温度

100 °C

A glass microwave reaction vessel was charged with 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one (609) (31 mg, 0.12 mmol) and N-(tert-butyl)-5-chloro-2-methylpyrido[3,4-b]pyrazin-3-amine (15 mg, 0.06 mmol) in 1,4-Dioxane (0.8 mL)/Water (0.2 mL) followed by Xphos (2.8 mg, 6.0 μmol) (Sigma Aldich), Pd2dba3 (2.7 mg, 3.0 μmol) (Strem) and K2PO4 (38 mg, 0.18 mmol) (Sigma Aldich). The reaction mixture was stirred and heated in an Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc., Upssala, Sweden) at 100° C. for 1 h. The mixture was diluted with CHCl3/iPrOH (4:1, 30 mL) and washed with water. The organic layer was dried (MgSO4), filtered and concentrated. The residue was purified with prep-TLC (eluted with 8% MeOH in DCM) to give 2-(3-(tert-butylamino)-2-methylpyrido[3,4-b]pyrazin-5-yl)-6,7-dihydro-1H-pyrrolo[3,2-c]pyridin-4(5H)-one (5.0 mg, 0.014 mmol, 24% yield) as a light brown solid. MS (ESI, pos. ion) m/z: 351.1 (M+1); 1H NMR (400 MHz, MEOH-D4-d4) δ ppm 8.33 (1H, d, J=5.5 Hz), 7.79 (1H, s), 7.45 (1H, d, J=5.5 Hz), 3.62 (2H, t, J=7.0 Hz), 3.01 (2H, t, J=7.0 Hz), 2.62 (3H, s), 1.70 (9H, s).

1. customA glass microwave reaction vessel
2. washwashed with water
3. dry with materialThe organic layer was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified with prep-TLC (eluted with 8% MeOH in DCM)