HRID1199796

反应详情

EQUATION

反应方程式

HRID 1199796 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 24 g (0.1199 mol) of the compound of (B), 15 ml (12.78 g/0.1796 mol) of pyrrolidine, 240 mg of p-toluenesulfonic acid, and 100 ml of benzene is stirred at reflux with the azeotropic removal of water for 6 hours. After cooling, the resulting precipitate is collected and triturated with ethyl ether to afford 20 (66%) of title compound: m.p. 126°-129° C.; IR (KBr) 2200, 1635, and 1600 cm-1 ; NMR (CDCl3) δ7.48 (d, 2H), 6.7 (d, 2H), 4.3-4.1 (m, 1H) 3.95-3.45 (m, 4H), 3.2-2.85 (m, 4H) 2.65-2.25 (m, 2H), and 1.95-1.75 (m, 4H).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe resulting precipitate is collected
  3. customtriturated with ethyl ether