HRID1199638
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 24 g (0.0947 mol) of the compound of (b), 12 ml (10.2 g/0.143 mol) of pyrrolidine, 240 mg of p-toluenesulfonic acid and 150 ml of benzene is heated at reflux with the azeotropic removel of water for 6 hours. After cooling the resulting precipitate is collected and triturated with ethyl ether to afford 22.5 g (78%) of title compound: m.p. 141°-143° C.; IR (KBr) 1650, 1580, 1300, and 1130 cm-1 ; NMR (CDCl3)δ 7.75 (d, 2H), 6.85 (d, 2H), 4.30-4.10 (m, 1H), 3.95-3.45 (m, 4H), 3.25-2.85 (m, 4H) 3.05 (s, 3H), 2.65-2.30 (m, 2H), and 1.95-1.70 (m, 4H).
WORKUP
后处理
- temperatureAfter cooling the resulting precipitate
- customis collected
- customtriturated with ethyl ether