反应详情

To a solution of 3-morpholin-4-yl-3-oxopropanenitrile (3.0 g, 19.5 mmol) in anhydrous THF (45 mL) was added Lawesson's reagent (4.2 g, 10.3 mmol). The reaction mixture was allowed to stir at rt for 16 h and was then concentrated to small volume. A solid precipitated and was filtered. The solid was washed with diethyl ether to give 3-morpholin-4-yl-3-thioxopropanenitrile (2.3 g, 70%). LCMS: (AA) ES+ 171.2. 1H NMR (400 MHz, CDCl3) δ: 4.27-4.29 (m, 2H), 4.00 (s, 2H) and 3.81-3.83 (m, 6H).

1. concentrationwas then concentrated to small volume
2. customA solid precipitated
3. filtrationwas filtered
4. washThe solid was washed with diethyl ether