반응 #68819

반응 방정식

Et3N

2-Methanesulfonyl-5-phenylethynyl-pyrimidine

methylamine hydrochloride

→

methyl-(5-phenylethynyl-pyrimidin-2-yl)-amine

용매

THF

반응 조건

후처리

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

실험 절차

(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+).

출처