HRID487389

反应详情

EQUATION

反应方程式

HRID 487389 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-amino-2,6-diethylpyridine-3-carbaldehyde (1.78 g), diethylmalonate (1.92 g), ethanol (15 ml) and piperidine (4 drops) were heated at reflux for 16 hours. Volatile material was removed by evaporation and the residue was recrystallised from ethyl acetate/petroleum ether to give ethyl 5,7-diethyl-2-oxo-1,2-dihydro-1,6-naphthyridine-3-carboxylate (B) (1.4 g), m.p. 159°-160° C.; NMR (CDCl3): 1.34(t, 3H), 1.38(t, 3H), 1.47(t, 3H), 2.87(q, 2H), 3.14(q, 2H), 4.47(q, 2H), 7.03(s, 1H), 8.78(s, 1H), 12.2(s, 1H); mass spectrum (CI, ammonia): 275 (M+H)+ ; microanalysis, found: C, 65.8; H, 6.8; N, 10.4%; C15H18N2O3 requires: C, 65.7; H, 6.6; N, 10.2%.

WORKUP

后处理

  1. temperatureat reflux for 16 hours
  2. customVolatile material was removed by evaporation
  3. customthe residue was recrystallised from ethyl acetate/petroleum ether