反応 #709368

反応方程式

hydrochloric acid

1-hydroxypyrazole

potassium carbonate

Carbon dioxide

→

1-hydroxypyrazole-4-carboxylic acid

収率 45.0%

溶媒

water

反応条件

後処理

1. 1
   workup.ADDITIONthe mixture is introduced into an autoclave
2. 2
   その他is forced in at room temperature until the pressure
3. 3
   温度after which heating
4. 4
   その他precipitates the 1-hydroxypyrazole-4-carboxylic acid
5. 5
   ろ過the latter is filtered off
6. 6
   その他recrystallized from water

実験手順

1 part of 1-hydroxypyrazole is mixed thoroughly with 4 parts of potassium carbonate, and the mixture is introduced into an autoclave. Carbon dioxide is forced in at room temperature until the pressure reaches 50 bar, after which heating is carried out for 20 hours at 150° C. The reactor content is then dissolved in water, the solution is acidified with hydrochloric acid, which precipitates the 1-hydroxypyrazole-4-carboxylic acid, and the latter is filtered off and recrystallized from water. 0.68 part (45% of theory) of 1-hydroxypyrazole-4-carboxylic acid of melting point 230° C. is obtained.

出典