反应详情

A mixture of NaOEt (0.074 mol) in EtOH (prepared from 1.7 g of Na and 75 mL of EtOH), acetamidine hydrochloride (3.5 g, 0.037 mol), and diethyl 2-trifluoroacetylsuccinate (10.0 g, 0.037 mol) was heated under reflux for 20 h. The mixture was concentrated, taken up in water, acidified to pH 4 with conc. HCl, and extracted with EtOAc. The extracts were washed with brine, dried (MgSO4), and concentrated to give an oily solid. Trituration with ether/hexane gave 2.63 g (27%) of product as a white solid. An analytical sample was recrystallized from ether/hexane, mp 108°-110° C.

1. temperaturewas heated
2. temperatureunder reflux for 20 h
3. concentrationThe mixture was concentrated
4. extractionextracted with EtOAc
5. washThe extracts were washed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customto give an oily solid