反应详情

Slurry 4-bromophenacyl bromide (11.2 g, 50 mmol) in absolute ethanol (50 mL). Add N-cyclopropylmethyl-thiourea (6.5 g, 50 mmol) and sodium bicarbonate (4.2 g, 50 mmol), heat to reflux for 2 h, then stir at room temperature overnight. Concentrate to ¼ volume and partition between water/EtOAc (4:1, 500 mL). Extract the aqueous layer with EtOAc (2×75 mL). Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to obtain the title compound (14.0 g, 91%) as an off-white solid that was used without further purification. MS (ES+) m/z: 310 (M+H)+.

1. temperatureto reflux for 2 h
2. concentrationConcentrate
3. custompartition between water/EtOAc (4:1, 500 mL)
4. extractionExtract the aqueous layer with EtOAc (2×75 mL)
5. dry with materialDry the combined organic extracts over Na2SO4
6. filtrationfilter
7. concentrationconcentrate in vacuo