HRID580599

反应详情

EQUATION

反应方程式

HRID 580599 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Sodium hydroxide (0.5 ml of 2N) was added to a mixture of trimethoxyacetophenone (2.1 g, 0.01 mole), dimethylaminobenzaldehyde (1.49 g, 0.01 mole), and ethanol (50 ml). The reaction mixture was allowed to stir at room temperature until a thin layer chromatography (50% ethyl acetate in hexane) indicated that the reaction was complete. After cooling to about 0° C., the mixture was filtered, the solid residue washed with water, then with methanol. Recrystallization from methanol gave the title compound, m.p. 145°-146° C. Elemental analysis for C20H23NO4 : Calcd: C, 70.36; H, 6.79; N, 4.10%. Found: C, 70.21; H, 6.98; N, 3.83%. Also prepared by substantially the same procedure as in example 2 were:

WORKUP

后处理

  1. filtrationthe mixture was filtered
  2. washthe solid residue washed with water
  3. customRecrystallization from methanol