反応 #82151

反応方程式

acyl azide

2-(4'-ethylenedioxy-1'-methyl-2'-oxocyclohexyl)-phenylacetyl azide

dimethylformamide

acetic acid

→

2-(2', 4'-dioxo-1'-methyl-cyclohexyl)-benzyl amine

反応条件

後処理

1. 1
   温度The solution is cooled

実験手順

The acyl azide 5 is dissolved in dimethylformamide and heated to 100° C. until nitrogen evolution ceases. The solution is cooled and treated with aqueous acetic acid to form 2-(2', 4'-dioxo-1'-methyl-cyclohexyl)-benzyl amine 6. Diethyl ether is added and the solution is washed successively with saturated sodium bicarbonate solution, water, and saturated salt solution and dried over anhydrous sodium sulfate. The solvent is removed by rotoevaporation to yield 1,2,3,4,4a,5,6,10b-octahydro- 10b-methyl-3-phenanthridinone 7.

出典