반응 #2438556

반응 방정식

2-amino-5-ethyl-N-(2-chloropyridin-3-yl)benzamide

acetonitrile

dichloromethane ethyl acetate

→

5,11-Dihydro-8-ethyl-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

용매

sulpholane

반응 조건

후처리

1. 1
   workup.WAITThe mixture was left
2. 2
   온도to cool
3. 3
   여과filtered
4. 4
   세척washed successively with 50 ml acetonitrile and 100 ml conc. ammonia
5. 5
   기타It was recrystallised from hot 70% acetic acid
6. 6
   기타after drying in a circulating air dryer 114.0 g (48% of theory) of pale yellow crystals
7. 7
   기타were obtained

실험 절차

160.0 g (0.58 mol) of the 2-amino-5-ethyl-N-(2-chloropyridin-3-yl)benzamide obtained were dissolved in 256 ml of sulpholane and heated to 170° C. with stirring for 20 minutes. The mixture was left to cool, stirred with 1 liter of acetonitrile, the resulting crystal slurry was suction filtered and washed successively with 50 ml acetonitrile and 100 ml conc. ammonia. It was recrystallised from hot 70% acetic acid and after drying in a circulating air dryer 114.0 g (48% of theory) of pale yellow crystals were obtained, m.p. 232°-234° C., RF 0.78 (Macherey-Nagel, PolygramRSIL G/UV254, pre-coated plastic sheets for TLC, eluant: dichloromethane/ethyl acetate 1/1 v/v).

출처