反应 #81835

反应方程式

5-acetyl-2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one

nitronium tetrafluoroborate

→

title compound

收率 18.6%

5-Acetyl-2-chloro-5,11-dihydro-11-ethyl-4-methyl-3-nitro-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one

收率 18.6%

溶剂

acetonitrile

反应条件

后处理

1. 1
   其他The mixture was removed from the ice bath
2. 2
   其他The reaction
3. 3
   其他then was quenched with 10% potassium carbonate
4. 4
   workup.ADDITIONEthyl acetate was added
5. 5
   其他the organic phase was separated
6. 6
   洗涤washed
7. 7
   其他dried
8. 8
   其他evaporated

实验过程

To a solution of 5-acetyl-2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (3.36 g) in acetonitrile (20 mL) cooled on ice was added nitronium tetrafluoroborate (85%, 2.26 g). The mixture was removed from the ice bath and was stirred for 5 hours. The reaction then was quenched with 10% potassium carbonate. Ethyl acetate was added and the organic phase was separated, washed, dried, and evaporated. Chromatography over silica gel gave 0.71 g of the title compound, which crystallized from diisopropyl ether, m.p. 140-141.

来源