反応 #1483037

反応方程式

nicotinic acid

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

EDCI

→

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

収率 56.0%

溶媒

CH3CN

EtOAc

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   洗浄The organic layer was washed with dilute aqueous NaHCO3, brine
3. 3
   乾燥dried over Na2SO4
4. 4
   ろ過filtered
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他Purification by silica gel chromatography (CH2Cl2)

実験手順

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%).

出典