反应详情

To a suspension of NaOH (68.44 g 1.71 mol, Aldrich, 20-40 mesh beads) in 171 mL of DMSO a solution of benzyl-2-nitrophenyl ether (39.23 g, 0.171 mol) and (phenylthio)acetonitrile (25.54 g, 0.171 mol, Lancaster) in 171 mL of DMSO was added dropwise for 10 min and stirred at r.t. for another 25 min. A mixture of 430 g of ice and 430 g of conc. HCl was added. The product precipitated and crystallized. The reaction mixture was cooled down in a refrigerator and filtered. The precipitate was dried on air (hood!) and recrystallized from EtOAc-hexanes. Yield 32.03 g (70%), mp 78-80° C.

1. additionwas added dropwise for 10 min
2. additionwas added
3. customThe product precipitated
4. customcrystallized
5. temperatureThe reaction mixture was cooled down in a refrigerator
6. filtrationfiltered
7. customThe precipitate was dried on air (hood!)
8. customrecrystallized from EtOAc-hexanes