HRID362697
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Diethyl 1-Acetyl-3-ethylpyrrolidine-2,2-dicarboxylate (373 g, 0.95 mol) was suspended in 6N HCl (2 L) and HOAc (500 mL) and heated at reflux for 20 h. The reaction mixture was cooled, washed with EtOAc (1L), then concentrated in vacuo to give an oil which crystallized upon trituration with ether to give the title compound. 1H NMR (D2O) δ 4.23 (d, 1H, J=8 Hz), 3.84 (d, 1H, J=8 Hz), 3.15-3.4 (m, 4H), 2.33-2.44 (m, 1H), 2.19-2.4 (m, 1H), 2.02-2.15 (m, 2H), 1.53-1.72 (m, 3H), 1.23-1.43 (m, 2H), 1.0-1.15 (m, 1H), 0.75-0.83 (m, 6H).
WORKUP
后处理
- temperatureat reflux for 20 h
- temperatureThe reaction mixture was cooled
- washwashed with EtOAc (1L)
- concentrationconcentrated in vacuo
- customto give an oil which
- customcrystallized upon trituration with ether