تفاعل #42790

معادلة التفاعل

N-acetylethylenediamine

2,6-dichloro-3-nitropyridine

N,N-diisopropylethylamine

→

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

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto warm to room temperature
2. 2
   workup.STIRRINGstirred for 72 hours
3. 3
   أخرىThe solvent was removed in vacuo
4. 4
   أخرىthe residue was purified by flash chromatography
5. 5
   غسيلeluting with MeOH/dichloromethane gradient (1→10%)

الإجراء التجريبي

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.

المصدر