反应详情

A solution of 4-(5-chloro-2-(6-methoxypyridin-3-ylamino)pyridin-3-yl)-N,N-bis(4-methoxybenzyl)-6-methyl-1,3,5-triazin-2-amine (110 mg, 0.188 mmol) in TFA (10 mL) was heated at 80° C. for 16 h. The orange mixture was concentrated to a slurry, diluted with saturated NaHCO3 (5 mL), and filtered. The solid was washed with water, MeOH, and (3:1) hexane-EtOAc to give the product as a brown solid (65 mg). LCMS (ES, pos.): calcd for C15H14ClN7O: 343.1. found: 344.1 (M+H)+. 1H NMR (400 MHz, d6-DMSO) δ 11.69 (br. s., 1H); 8.72 (br. s., 1H); 8.50 (d, J=3.33 Hz, 1H); 8.31 (br. s., 1H); 8.09 (br. s., 1H); 7.94 (br. s., 1H); 7.80 (br. s., 1H); 6.84 (br. s., 2H); 3.85 (br. s., 3H); 2.43 (br. s., 3H).

1. concentrationThe orange mixture was concentrated to a slurry
2. additiondiluted with saturated NaHCO3 (5 mL)
3. filtrationfiltered
4. washThe solid was washed with water, MeOH, and (3:1) hexane-EtOAc