반응 #336843

반응 방정식

hydrochloric acid

sodium hydroxide

diethyl oxalacetate sodium salt

4-Chlorobenzenecarboximidamide monohydrochloride

→

title compound

수율 45.0%

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

수율 45.0%

용매

water

반응 조건

후처리

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

실험 절차

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).

출처