反应详情

温度

22 °C

A 5-L 3-neck flask equipped with an overhead mechanical stirrer, N2 inlet/outlet adapter, and thermocouple was charged with 4M HCl in 1,4-dioxane (3.1 L), tert-butyl-3-methylbenzo[b]thiophen-2-ylcarbamate (265 g, 1.0 mol) and stirred for 18 h at 22° C. The resulting white precipitate was collected by filtration, washed with diethyl ether (3×500 mL), and dried under house vacuum at 40° C. for 48 h to yield 3-methylbenzo[b]thiophen-2-amine hydrochloride as a white solid. 1H-NMR (DMSO-d6) δ 8.7 (br s, 3H), 7.71 (d, 1H), 7.44 (d, 1H), 7.29 (t, 1H), 7.14 (t, 1H), 2.184 (s, 3H).

1. customA 5-L 3-neck flask equipped with an overhead mechanical stirrer, N2 inlet/outlet adapter
2. filtrationThe resulting white precipitate was collected by filtration
3. washwashed with diethyl ether (3×500 mL)
4. customdried under house vacuum at 40° C. for 48 h