반응 #42790

반응 방정식

N-acetylethylenediamine

2,6-dichloro-3-nitropyridine

N,N-diisopropylethylamine

→

N-(2-(6-chloro-3-nitropyridin-2-ylamino)ethyl)acetamide

용매

THF

반응 조건

후처리

1. 1
   온도to warm to room temperature
2. 2
   workup.STIRRINGstirred for 72 hours
3. 3
   기타The solvent was removed in vacuo
4. 4
   기타the residue was purified by flash chromatography
5. 5
   세척eluting with MeOH/dichloromethane gradient (1→10%)

실험 절차

To a solution of 3.0 g (15.5 mmol) 2,6-dichloro-3-nitropyridine in 50 mL of THF at −78° C. under Ar atmosphere was added 2.7 mL (15.5 mmol) of N,N-diisopropylethylamine followed by 1.6 mL (15.5 mmol) of N-acetylethylenediamine. The mixture was stirred at −78° C. for 30 min, allowed to warm to room temperature, and stirred for 72 hours. The solvent was removed in vacuo and the residue was purified by flash chromatography eluting with MeOH/dichloromethane gradient (1→10%) to provide N-(2-(6-chloro-3-nitropyridin-2-ylamino)ethyl)acetamide as pale yellow solid.

출처