反应 #42782

反应方程式

7-(4-chlorophenyl)-6-isopropyl-2,3-dihydro-1H-1-aza-4,5-dioxa-phenanthren-8-one

N,N-dimethylformamide

→

title compound

4-(6-Isopropyl-8-oxo-1,2,3,8-tetrahydro-4,5-dioxa-1-aza-phenanthren-7-yl)benzonitrile

反应条件

后处理

1. 1
   过滤The mixture is filtered through a short pad of Celite, which
2. 2
   洗涤is then thoroughly washed through with ethyl acetate
3. 3
   洗涤The filtrate is washed successively with water and brine
4. 4
   干燥The organic layer is dried (MgSO4)
5. 5
   浓缩concentrated in vacuo
6. 6
   其他The residue is purified by flash chromatography (cyclohexane/ethyl acetate gradient)

实验过程

A mixture of 7-(4-chlorophenyl)-6-isopropyl-2,3-dihydro-1H-1-aza-4,5-dioxa-phenanthren-8-one (71.7 mg, 0.202 mmol), tris(dibenzylideneacetone)dipalladium (0) (92.2 mg, 0.101 mmol), 1,1′-bis(diphenylphosphino)ferrocene (112 mg, 0.202 mmol) and zinc cyanide (24 mg, 0.204 mmol) in N,N-dimethylformamide (2.5 ml) is heated at 180° C. for 40 min under microwave irradiation in an Emrys Optimizer instrument (Biotage AB, Uppsala, Sweden). The mixture is filtered through a short pad of Celite, which is then thoroughly washed through with ethyl acetate. The filtrate is washed successively with water and brine. The organic layer is dried (MgSO4) and concentrated in vacuo. The residue is purified by flash chromatography (cyclohexane/ethyl acetate gradient) to afford the title compound.

来源