HRID1614290

反应详情

EQUATION

反应方程式

HRID 1614290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 3-piperidinecarboxylic acid, 2,4-dioxo-, methyl ester, ion (1-), sodium (10.0 g) in water (24 ml) and 2M aqueous hydrochloric acid (26 ml) was heated at reflux for 30 min. The resulting mixture was cooled to ca. 20°, diluted with industrial methylated spirit (25 ml) and treated with 1-methyl-1-phenylhydrazine sulphate (2:1) (8.8 g) and 5M aqueous sodium hydroxide (12 ml). The resulting suspension was diluted with water (25 ml), cooled to ca. 0° and filtered to give the title compound (9.1 g), m.p. 185°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 30 min
  3. temperatureThe resulting mixture was cooled to ca. 20°
  4. temperaturecooled to ca. 0°
  5. filtrationfiltered