反应 #336843

反应方程式

hydrochloric acid

sodium hydroxide

diethyl oxalacetate sodium salt

4-Chlorobenzenecarboximidamide monohydrochloride

→

title compound

收率 45.0%

2-(4-chlorophenyl)-1,6-dihydro-6-oxo-4-pyrimidinecarboxylic acid

收率 45.0%

溶剂

water

反应条件

后处理

1. 1
   workup.DISSOLUTIONAfter 1 h the solids had dissolved
2. 2
   workup.ADDITIONwas slowly added (causing foaming) until the pH
3. 3
   其他The solid was isolated by filtration
4. 4
   洗涤washed with water and methanol
5. 5
   其他The solid was then triturated twice with hot methanol
6. 6
   洗涤washed repeatedly with 1 N hydrochloric acid
7. 7
   干燥once with methanol and dried

实验过程

To a mixture of diethyl oxalacetate sodium salt (123.2 g, 586 mmol) in water (750 mL) was slowly added aqueous sodium hydroxide (50%, 47 g, 586 mmol). After 1 h the solids had dissolved. 4-Chlorobenzenecarboximidamide monohydrochloride (111.95 g, 586 mmol) was then added, and the mixture was heated at 70° C. overnight. After cooling to room temperature concentrated hydrochloric acid was slowly added (causing foaming) until the pH was lowered to 1.5. The solid was isolated by filtration and washed with water and methanol. The solid was then triturated twice with hot methanol, washed repeatedly with 1 N hydrochloric acid, then once with methanol and dried to afford the title compound (66.07 g).

来源