反应详情

A solution of tert-butyl 4-((5-(4-(bis(4-methoxybenzyl)amino)-6-methyl-1,3,5-triazin-2-yl)-6-(5-fluoro-6-methoxypyridin-3-ylamino)pyridin-3-yl)methyl)piperazine-1-carboxylate (25 g, 32.6 mmol) in dichloromethane (150 mL, 32.6 mmol) and trifluoroacetic acid (150 mL, 2019 mmol) was stirred at room temperature for 1 h. The solution was concentrated and the residue was dissolved in DCM and carefully neutralized with saturated aqueous NaHCO3. The aqueous layer was extracted with DCM and the organic extracts were dried over Na2SO4, filtered and concentrated in vacuo to give 4-(2-(5-fluoro-6-methoxypyridin-3-ylamino)-5-(piperazin-1-ylmethyl)pyridin-3-yl)-N,N-bis(4-methoxybenzyl)-6-methyl-1,3,5-triazin-2-amine (20 g, 30.0 mmol, 92% yield). The crude product was taken on to the next step without purification.

1. concentrationThe solution was concentrated
2. dissolutionthe residue was dissolved in DCM
3. extractionThe aqueous layer was extracted with DCM
4. dry with materialthe organic extracts were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo