反应详情

温度

100 °C

A mixture of benzyl 3-[4-amino-5-(2-benzyl-2H-indazol-6-yl)pyrrolo[2,1-f][1,2,4]triazin-7-yl]azetidine-1-carboxylate (304 mg, 0.57 mmol) and 6N aqueous HCl (10 mL) were stirred at 100° C. for 1 h. The mixture was concentrated to dryness. The residue was purified by preparative HPLC using a gradient elution from 15% to 50% 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 26 mg (11%) of the desired product, which was approximately 70% pure. ES-MS m/z 396.42 [M+H]+, HPLC RT (min) 2.04.

1. concentrationThe mixture was concentrated to dryness
2. customThe residue was purified by preparative HPLC
3. washa gradient elution from 15% to 50% acetonitrile in water
4. filtrationfollowed by filtration through an acidic resin
5. washwashing with MeOH
6. washThe product was eluted with 2M NH3 in MeOH
7. concentrationthe filtrate was concentrated