反应详情

A mixture of the title compound of Example 41 (0.684 g, 2.0 mmol), N-tert-butoxycarbonyl glycine (0.368 g, 2.1 mmol), N,N-dimethylaminopyridine (0.049 g, 0.4 mmol), dimethylformamide (15 ml), and N,N-diisopropylcarbodiimide (0.278 g, 2.2 mmol) was stirred for 12 hours. The mixture was concentrated under reduced pressure. The residue was purified by flash chromatography eluting with 40% ethyl acetate-hexane to provide 2-tert-butoxycarbonylamino-acetic acid 4-[4-amino-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2yl-amino]-benzyl ester (1.05 g, 100% yield). 1H NMR (CDCl3) δ 7.74 (s, 1H), 7.63-7.74 (d, 1H), 7.6 (br s, 2H), 7.31-7.36 (m, 4H), 7.20-7.22 (d, 1H), 5.3-5.6 (br s, 2H), 5.17 (d, 2H) 4.95-5.1 (br s, 1H), 3.965 (d, 2H), 2.55 (s, 3H), 1.47 (s, 9H).

1. concentrationThe mixture was concentrated under reduced pressure
2. customThe residue was purified by flash chromatography
3. washeluting with 40% ethyl acetate-hexane