反应 #45702

反应方程式

4-(Benzyloxycarbonylamino)butyric acid

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

1-hydroxybenzotriazole

dimethylamine

→

solid

收率 82.5%

Benzyl (3-dimethylcarbamoylpropyl)carbamate

收率 82.5%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   其他The reaction liquid
2. 2
   浓缩was concentrated under reduced pressure
3. 3
   workup.ADDITIONdiluted with ethyl acetate
4. 4
   洗涤washed with water
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   其他The solvent was evaporated away under reduced pressure
7. 7
   其他the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=70:1 to 40:1)

实验过程

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%).

来源