反应 #1483037
ord-cac4422a47934e218893df834988383c
反应方程式
nicotinic acid
tert-butyl 2-(2-(2-aminoethyl)disulfanyl)ethylcarbamate
EDCI
→
tert-butyl 2-(2-(2-(nicotinamido)ethyl)disulfanyl)ethylcarbamate
收率 56.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他The resulting reaction mixture
- 2洗涤The organic layer was washed with dilute aqueous NaHCO3, brine
- 3干燥dried over Na2SO4
- 4过滤filtered
- 5浓缩concentrated under reduced pressure
- 6其他Purification by silica gel chromatography (CH2Cl2)
实验过程
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%).