反应详情

A solution of ethyl 3-(t-butylthio)-2-oxopropanoate (18.6 g), 1-(4-chlorobenzyl)-1-(4-allyloxyphenyl)hydrazine hydrochloride (26.3 g), and NaOAc (15 g) in 300 mL toluene and 150 mL HOAc was stirred at room temperature under nitrogen for 16 hours then at 70° C. for 2 hours. The mixture was cooled, poured onto H2O, extracted (3×) with EtOAc and, the organic layers then washed successively with sat'd. NaHCO3 and brine. After drying over MgSO4, the solution was filtered and evaporated, and the residue chromatographed (silica gel; hexane/EtOAc 4:1) to afford the title compound.

1. temperatureThe mixture was cooled
2. additionpoured onto H2O
3. extractionextracted (3×) with EtOAc
4. washthe organic layers then washed successively with sat'd
5. dry with materialAfter drying over MgSO4
6. filtrationthe solution was filtered
7. customevaporated
8. customthe residue chromatographed (silica gel; hexane/EtOAc 4:1)