HRID362697

反应详情

EQUATION

反应方程式

HRID 362697 的结构方程式

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

  1. temperatureat reflux for 20 h
  2. temperatureThe reaction mixture was cooled
  3. washwashed with EtOAc (1L)
  4. concentrationconcentrated in vacuo
  5. customto give an oil which
  6. customcrystallized upon trituration with ether