HRID1614290
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 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
- temperaturewas heated
- temperatureat reflux for 30 min
- temperatureThe resulting mixture was cooled to ca. 20°
- temperaturecooled to ca. 0°
- filtrationfiltered