반응 #7007

반응 방정식

1-hydroxybenzotriazole hydrate

3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride

Butyric acid hydrazide

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

→

title compound

수율 62.0%

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

수율 62.0%

용매

dichloromethane

dichloromethane

sodium hydrogen carbonate

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   농축The reaction mixture was concentrated under reduced pressure
3. 3
   기타the solid formed
4. 4
   기타was isolated by filtration
5. 5
   기타The material obtained
6. 6
   기타was dried under vacuum at 40° C.

실험 절차

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).

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