反应详情

温度

65 °C

(100 mg, 0.38 mmol) 2-Methanesulfonyl-5-phenylethynyl-pyrimidine (Example 8, step 2), methylamine hydrochloride (52 mg, 0.77 mmol, 2 equiv.) and Et3N (220 μl, 1.55 mmol, 4 equiv.) were suspended in 1 ml THF and stirred for 1 hour at 65° C. The reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography by directly loading the crude material onto a silica gel column and eluting with (heptane:ethyl acetate 100:0->0:100). The desired methyl-(5-phenylethynyl-pyrimidin-2-yl)-amine was obtained as a white solid (38 mg, 47%), MS: m/e=210.2 (M+H+).

1. concentrationThe reaction mixture was concentrated in vacuo
2. customthe residue was purified by flash chromatography
3. washeluting with (heptane:ethyl acetate 100:0->0:100)