تفاعل #45702

معادلة التفاعل

4-(Benzyloxycarbonylamino)butyric acid

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

1-hydroxybenzotriazole

dimethylamine

→

solid

المردود 82.5%

Benzyl (3-dimethylcarbamoylpropyl)carbamate

المردود 82.5%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction liquid
2. 2
   تركيزwas concentrated under reduced pressure
3. 3
   workup.ADDITIONdiluted with ethyl acetate
4. 4
   غسيلwashed with water
5. 5
   تجفيفdried over anhydrous sodium sulfate
6. 6
   أخرىThe solvent was evaporated away under reduced pressure
7. 7
   أخرىthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=70:1 to 40:1)

الإجراء التجريبي

4-(Benzyloxycarbonylamino)butyric acid (0.74 g, 3.12 mmol) was dissolved in N,N-dimethylformamide, then 1-(dimethylaminopropyl)-3-ethylcarbodiimide 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.60 g, 3.13 mmol), 1-hydroxybenzotriazole (0.48 g, 3.13 mmol) and dimethylamine (2.0 M tetrahydrofuran solution, 2.40 ml, 4.80 mmol) were added, followed by stirring at room temperature for 3 days. The reaction liquid was concentrated under reduced pressure, diluted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=70:1 to 40:1) to obtain a yellow solid (0.68 g, 82%).

المصدر