反应详情

A solution of 1-(5-cyano-pyrazin-2-yl)-3-[5-methyl-2-(morpholin-2-ylmethoxy)-phenyl]-urea hydrochloride salt (0.0104 g, 0.129 mmol) in MeOH (1 mL) was cooled to 0° C. and treated with an aqueous solution of formaldehyde (0.12 mmol) followed by sodium triacetoxy borohydride (0.06 g, 0.292 mmol). The reaction was stirred for 12 h, then concentrated in vacuo. The residue was chromatographed on silica (2% MeOH in CH2Cl2) to give the product as a white solid (0.014 g). 1H-NMR (400 MHz, d6-DMSO) δ 10.90 (s, 1, H), 10 (br s, 1, H), 8.9 (s, 1, H), 8.8 (s, 1, H), 8 (s, 1, H), 6.9 (m, 1, H), 6.8 μm, 1, H), 3.9 (m, 4, H), 3.6 (t, 1, H), 2.9 (d, 1, H), 2.7 (d, 1, H), 2.2 (s, 3, H), 2.1 (s, 3, H), 2 (t, 1, H), 1.8 (t, 1, H). LRMS (esi, positive) m/e 383.40 (M+1).

1. concentrationconcentrated in vacuo
2. customThe residue was chromatographed on silica (2% MeOH in CH2Cl2)