反应详情

56.3 g of sodium methanolate were taken up in 1 l of DMSO and, at RT, 56.3 ml of nitromethane were added dropwise. The internal temperature rose to 40° C. during this. Then, at a temperature between 26° C. and 30° C., a solution of 145.0 g of phenyl 2-(4-fluorophenyl)ethenesulfonate in 1 l of DMSO was added dropwise. Stirring at RT for 1 hour was followed by leaving to stand at RT for 16 hours and then stirring at RT for a further 6 hours and 30 minutes. The reaction mixture was then poured into 8 kg of ice and extracted 5 times with 2 l of EA each time. After drying over Na2SO4, the solvent was removed in vacuo. Chromatography on silica gel with EA/HEP 1:5 afforded 77.35 g of a colorless oil.

1. customrose to 40° C.
2. customby leaving
3. waitto stand at RT for 16 hours
4. stirringstirring at RT for a further 6 hours and 30 minutes
5. extractionextracted 5 times with 2 l of EA each time
6. dry with materialAfter drying over Na2SO4
7. customthe solvent was removed in vacuo