反应 #1483038

反应方程式

tert-Butyl 2-(2-aminoethoxy)ethylcarbamate

nicotinic acid

EDCI

→

tert-butyl 2-(2-(nicotinamido)ethoxy)ethylcarbamate

收率 44.0%

溶剂

CH3CN

EtOAc

反应条件

后处理

1. 1
   其他The resulting reaction mixture
2. 2
   洗涤washed with saturated aqueous NaHCO3, brine
3. 3
   干燥dried over Na2SO4
4. 4
   过滤filtered
5. 5
   浓缩concentrated under reduced pressure
6. 6
   其他The resulting residue was purified by silica gel chromatography (9:1 CH2Cl2/MeOH)

实验过程

tert-Butyl 2-(2-aminoethoxy)ethylcarbamate (420, 2.06 mmol) was then taken up in CH3CN (20 mL) along with nicotinic acid (253 mg, 2.06 mmol) and EDCI (434 mg, 2.3 mmol). The resulting reaction mixture was stirred at room temperature for 18 h. It was then diluted with EtOAc (20 mL), washed with saturated aqueous NaHCO3, brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (9:1 CH2Cl2/MeOH) to afford tert-butyl 2-(2-(nicotinamido)ethoxy)ethylcarbamate (280 mg, 44%). MS calculated for C15H23N3O4: 309.17. Found: [M+H]+ 310.

来源