反应详情

The combined compounds were taken up in CH2Cl2 (2 mL) TFA (4 mL) was added. The resulting mixture was stirred at RT for 4 h, upon which the volatiles were removed in vacuo. The residue was neutralized with sat. NaHCO3 and extracted with THF (3×25 mL). The combined organics were washed with brine (1×20 mL), dried (Na2SO4) and purified by preparative TLC (SiO2, CH2Cl2:MeOH:NH4OH 9:1:0.1). The purified compound was taken up in CH2Cl2 (2 mL) and HCl (4M in 1,4 dioxane, 10 mL) and was stirred at RT for 4 h. The volatiles were removed in vacuo and the residue was triturated with Et2O, filtered and dried under vacuum to give N-(3-(4-(1H-indazol-5-ylamino)-6-(2-(4-methylpiperazin-1-yl)ethoxy)quinazolin-2-yl)phenyl)butyramide di-hydrochloride salt (0.067 g, 0.105 mmol, 42% over two steps). MS 565 (M+1). HPLC retention time 4.30 mins.

1. additionwas added
2. customwere removed in vacuo
3. extractionextracted with THF (3×25 mL)
4. washThe combined organics were washed with brine (1×20 mL)
5. dry with materialdried (Na2SO4)
6. custompurified by preparative TLC (SiO2, CH2Cl2:MeOH:NH4OH 9:1:0.1)
7. stirringHCl (4M in 1,4 dioxane, 10 mL) and was stirred at RT for 4 h
8. customThe volatiles were removed in vacuo
9. customthe residue was triturated with Et2O
10. filtrationfiltered
11. customdried under vacuum