反应 #2467953

反应方程式

N-[2-(Acetylamino)propionyl]phenylalanine

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

1-hydroxybenzotriazole

piperidine

→

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

溶剂

N,N-dimethylformamide

water

反应条件

后处理

1. 1
   其他Fog 24 hours
2. 2
   萃取the resulting mixture is extracted three times with chloroform
3. 3
   洗涤The organic layer is washed with 10% hydrochloric acid
4. 4
   干燥a 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
   其他the residue is purified by silica gel column chromatography

实验过程

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.

来源