تفاعل #2467953

معادلة التفاعل

N-[2-(Acetylamino)propionyl]phenylalanine

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride

1-hydroxybenzotriazole

piperidine

→

1-{2-[N-(2-(acetylamino)propionyl)amino]-3-phenylpropionyl}piperidine

المذيبات

N,N-dimethylformamide

water

ظروف التفاعل

المعالجة

1. 1
   أخرىFog 24 hours
2. 2
   استخلاصthe resulting mixture is extracted three times with chloroform
3. 3
   غسيلThe organic layer is washed with 10% hydrochloric acid
4. 4
   تجفيفa saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONAfter the solvent is distilled away under reduced pressure
6. 6
   أخرىthe residue is purified by silica gel column chromatography

الإجراء التجريبي

N-[2-(Acetylamino)propionyl]phenylalanine obtained in Experimental Example 21 (10 mg, 0.036 mmol) is suspended in N,N-dimethylformamide (5 ml), and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (14 mg, 0.073 mmol), 1-hydroxybenzotriazole (15 mg, 0.11 mmol) and piperidine (40 μl, 0.40 mmol) are added to the suspension at room temperature, followed by stirring at 50° C. Fog 24 hours. To the reaction mixture is added water, and the resulting mixture is extracted three times with chloroform. The organic layer is washed with 10% hydrochloric acid and a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate. After the solvent is distilled away under reduced pressure, the residue is purified by silica gel column chromatography to obtain 1-{2-[N-(2-(acetylamino)propionyl)amino]-3-phenylpropionyl}piperidine.

المصدر