تفاعل #44979

معادلة التفاعل

2-amino-5-chloropyridine

triethylamine

Chloroacetyl chloride

→

title compound

2-Chloro-N-(5-chloropyridin-2-yl)acetamide

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONis added dropwise
2. 2
   درجة الحرارةcooling
3. 3
   تركيزThe reaction solution is concentrated under reduced pressure
4. 4
   workup.ADDITIONis poured ice-water
5. 5
   استخلاصfollowed by extraction with ethyl acetate
6. 6
   غسيلThe organic layer is washed with saturated brine
7. 7
   تجفيفdried over sodium sulfate
8. 8
   workup.ADDITIONtreated with activated charcoal
9. 9
   ترشيحAfter filtration
10. 10
    أخرىto remove insoluble materials
11. 11
    تركيزthe filtrate is concentrated under reduced pressure
12. 12
    ترشيحThe precipitates are collected by filtration
13. 13
    غسيلwashed with diisopropyl ether
14. 14
    أخرىdried

الإجراء التجريبي

Chloroacetyl chloride (95.5 ml) is dissolved in dichloromethane (500 ml), and thereto is added dropwise a suspension of 2-amino-5-chloropyridine (128.6 g) and triethylamine (169 ml) in dichloromethane (1000 ml) under ice-cooling. The reaction solution is warmed to room temperature and stirred for 0.5 hours. The reaction solution is concentrated under reduced pressure, and thereto is poured ice-water, followed by extraction with ethyl acetate. The organic layer is washed with saturated brine, dried over sodium sulfate and treated with activated charcoal. After filtration to remove insoluble materials, the filtrate is concentrated under reduced pressure and the resulting residue is suspended in diisopropyl ether. The precipitates are collected by filtration, washed with diisopropyl ether and dried to give the title compound (153.4 g).

المصدر