تفاعل #45704

معادلة التفاعل

Ethyl 3-aminopropionate hydrochloride

benzyl chloroformate

triethylamine

→

Ethyl 3-(benzyloxycarbonylamino)propionate

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   أخرىthe reaction, liquid
3. 3
   تركيزwas concentrated
4. 4
   workup.ADDITIONEthyl acetate and water were added
5. 5
   أخرىthe organic layer was collected
6. 6
   تجفيفdried over anhydrous sodium sulfate
7. 7
   أخرىThe solvent was evaporated away under reduced pressure
8. 8
   أخرىthe resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1)
9. 9
   أخرىto obtain a pale yellow oil (3.26 g, quant)

الإجراء التجريبي

Ethyl 3-aminopropionate hydrochloride (2.00 g, 13.0 mmol) was dissolved in dichloromethane (40 ml), and benzyl chloroformate (2.00 ml, 14.1 mmol) was added. With cooling with ice, triethylamine (4.00 ml, 28.9 mmol) was added, followed by stirring at room temperature for 15 hours, then the reaction, liquid was concentrated. Ethyl acetate and water were added, the organic layer was collected, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, the resulting residue was purified by silica gel column chromatography (dichloromethane to dichloromethane:methanol=70:1) to obtain a pale yellow oil (3.26 g, quant).

المصدر