反应详情

To 50.00 g (0.247 mol) of diethyl acetonedicarboxylate was added dropwise 31.79 g (0.297 mol) of benzylamine at such a rate that reaction temperature was kept below 50° C. The reaction mixture was stirred at room temperature for 12 hours and poured into H2O, extracted twice with ether, dried (MgSO4) and concentrated in vacuo affording 60.00 g of a yellow-green oil. Crude was purified by HPLC using 10% ethyl acetate/cyclohexane affording 46.2 g of a yellow semi solid. This was kugelrohr distilled at 53 Pa and collected at a pot temperature of 148°-150° C. to give 39.4 g (55%) of enamine diester as a beige crystalline solid; mp 34°-36° C.

1. customthat reaction temperature
2. customwas kept below 50° C
3. extractionextracted twice with ether
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo