反応 #337200
ord-222b19def4df4654a04767a99799547a
反応方程式
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1濃縮The mixture was concentrated in vacuo
実験手順
To 5-methoxypyridin-2-amine (5 g, 40 mmol) in dioxane (40 mL) was added ethoxycarbonyl isothiocyanate (5.23 mL, 44.3 mmol). The reaction mixture was stirred at room temperature overnight. The mixture was concentrated in vacuo to afford 5-methoxypyridin-2-amine ethoxycarbonyl thiourea (10.28 g, 40.3 mmol, 100% yield). 1H NMR (300 MHz, DMSO-d6) δ ppm 12.03 (1 H, br. s.), 11.37 (1 H, br. s.), 8.53 (1 H, br. s.), 8.11 (1 H, d, J=2.93 Hz), 7.50 (1 H, dd, J=8.97, 3.11 Hz), 4.22 (2 H, q, J=7.07 Hz), 3.84 (3 H, s), 1.26 (3 H, t, J=7.14 Hz). MS (LC/MS) R.T.=2.40; [M+H]+=256.1.