반응 #1483037

반응 방정식

nicotinic acid

tert-butyl 2-(2-(2-aminoethyl)disulfanyl)ethylcarbamate

EDCI

→

tert-butyl 2-(2-(2-(nicotinamido)ethyl)disulfanyl)ethylcarbamate

수율 56.0%

용매

CH3CN

EtOAc

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   세척The organic layer was washed with dilute aqueous NaHCO3, brine
3. 3
   건조dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated under reduced pressure
6. 6
   기타Purification by silica gel chromatography (CH2Cl2)

실험 절차

Separately, nicotinic acid (246 mg, 2.0 mmol) was taken up in CH3CN (10 mL) along with tert-butyl 2-(2-(2-aminoethyl)disulfanyl)ethylcarbamate (503 mg, 2.0 mmol), EDCI (422 mg, 2.2 mmol). The resulting reaction mixture was stirred at room temperature for 4 h and then diluted with EtOAc. The organic layer was washed with dilute aqueous NaHCO3, brine, dried over Na2SO4, filtered and concentrated under reduced pressure. Purification by silica gel chromatography (CH2Cl2) afforded tert-butyl 2-(2-(2-(nicotinamido)ethyl)disulfanyl)ethylcarbamate (400 mg, 56%).

출처