反应详情

A mixture of 5-(2-benzyl-2H-indazol-6-yl)-7-(1,2,3,6-tetrahydropyridin-4-yl)pyrrolo[2,1-f][1,2,4]triazin-4-amine (100 mg, 0.24 mmol), N,N-dimethylglycine (27 mg, 0.26 mmol), EDCl (50 mg, 0.26 mmol), HOBt (35 mg, 026 mmol), and N,N-diisopropylethylamine (124 μL, 0.71 mmol) in DMF (1.5 mL) was stirred at rt for 16 h. The crude mixture was purified by preparative HPLC using a gradient elution from 15% to 45% acetonitrile in water followed by filtration through an acidic resin, washing with MeOH. The product was eluted with 2M NH3 in MeOH and the filtrate was concentrated to provide 24 mg (20%) of the desired product. 1H NMR (400 MHz, DMSO-d6) δ 8.55 (s, 1 H), 7.96 (s, 1 H), 7.81 (d, 1 H), 7.61 (s, 1 H), 7.27-7.37 (m, 5 H), 7.14 (dd, 1 H), 7.03-7.10 (m, 1 H), 6.80-6.84 (m, 1 H), 5.65 (s, 2 H), 4.25 (d, 2 H), 3.69 (dt, 2 H), 3.13 (d, 2 H), 2.63-2.70 (m, 1 H), 2.53-2.60 (m, 1 H), 2.17 (m, 6 H); ES-MS m/z 507.17 [M+H]+, HPLC RT (min) 1.36.

1. customThe crude mixture was purified by preparative HPLC
2. washa gradient elution from 15% to 45% acetonitrile in water
3. filtrationfollowed by filtration through an acidic resin
4. washwashing with MeOH
5. washThe product was eluted with 2M NH3 in MeOH
6. concentrationthe filtrate was concentrated