反応 #2467953

反応方程式

N-[2-(Acetylamino)propionyl]phenylalanine

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

1-hydroxybenzotriazole

piperidine

→

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

溶媒

N,N-dimethylformamide

water

反応条件

後処理

1. 1
   その他Fog 24 hours
2. 2
   抽出the resulting mixture is extracted three times with chloroform
3. 3
   洗浄The organic layer is washed with 10% hydrochloric acid
4. 4
   乾燥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
   その他the residue is purified by silica gel column chromatography

実験手順

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.

出典