反应详情

温度

90 °C

To a solution of methylcyclopropyl bromide (4.00 g, 29.6 mmol) in ethanol (20.0 mL) was added potassium thiotosylate (10.0 g, 44.4 mmol) and the mixture heated to 90° C. for 10 h. The mixture was then quenched into a 1:1 mixture of H2O (50.0 mL) and diethyl ether (50.0 mL). The layers were separated and the organic layer washed with brine (50.0 mL). The organic layer was then dried with MgSO4 and concentrated in vacuo to yield the title compound as a solid (5.2 g, m.p. 46-48° C.). 1H NMR (400 MHz, CDCl3) δ7.816 (d, 2 H, J=8.8 Hz), 7.308 (d, 2 H, J =8.8 Hz), 2.945 (d, 2 H, J=7.6 Hz), 2.451 (s, 3 H), 1.010-0.933 (m, 1 H), 0.592-0.545 (m, 2 H), 0.236-0.197 (m, 2 H).

1. customThe mixture was then quenched into a 1:1 mixture of H2O (50.0 mL) and diethyl ether (50.0 mL)
2. customThe layers were separated
3. washthe organic layer washed with brine (50.0 mL)
4. dry with materialThe organic layer was then dried with MgSO4
5. concentrationconcentrated in vacuo