تفاعل #7007

معادلة التفاعل

1-hydroxybenzotriazole hydrate

3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride

Butyric acid hydrazide

1-pyrimidin-2-yl-piperidine-4-carboxylic acid

→

title compound

المردود 62.0%

1-Pyrimidin-2-yl-piperidine-4-carboxylic acid N′-butyryl-hydrazide

المردود 62.0%

المذيبات

dichloromethane

dichloromethane

sodium hydrogen carbonate

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   تركيزThe reaction mixture was concentrated under reduced pressure
3. 3
   أخرىthe solid formed
4. 4
   أخرىwas isolated by filtration
5. 5
   أخرىThe material obtained
6. 6
   أخرىwas dried under vacuum at 40° C.

الإجراء التجريبي

A mixture of 1-pyrimidin-2-yl-piperidine-4-carboxylic acid (3.0 g, 14.5 mmol)(see reference U.S. Pat. No. 4,826,843), 1-hydroxybenzotriazole hydrate (1.96 g, 14.5 mmol) and 1-(3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (2.78 g, 14.5 mmol) in dichloromethane (100 ml) was stirred for 10 minutes. Butyric acid hydrazide (1.78 g, 17.4 mmol) was added and the reaction mixture was stirred under a nitrogen atmosphere for 18 hours. The reaction mixture was diluted with dichloromethane (100 ml) and sodium hydrogen carbonate solution was added. The reaction mixture was concentrated under reduced pressure and the solid formed was isolated by filtration. The material obtained was dried under vacuum at 40° C. to give the title compound (2.62 g).

المصدر