反応 #81914

反応方程式

4-Piperidinylmethyl 8-amino-7-chloro-1,4-benzodioxan-5-carboxylate

acrylonitrile

→

title compound

収率 17.0%

[1-(2-Cyanoethyl)-4-piperidinyl]methyl 8-amino-7-chloro-1,4-benzodioxan-5-carboxylate

収率 17.0%

溶媒

acetone

反応条件

後処理

1. 1
   温度The solution was heated
2. 2
   温度at reflux (18 hours)
3. 3
   温度cooled
4. 4
   その他evaporated in vacuo to an orange gum
5. 5
   その他The gum was purified by flash silica-gel chromatography with CHCl3 →2% MeOH/CHCl3 as eluant

実験手順

4-Piperidinylmethyl 8-amino-7-chloro-1,4-benzodioxan-5-carboxylate (0.180 g, 0.55 mmol) was dissolved in acetone (10 ml) and treated with acrylonitrile (0.040 ml; 0.61 mmol). The solution was heated at reflux (18 hours), cooled and evaporated in vacuo to an orange gum. The gum was purified by flash silica-gel chromatography with CHCl3 →2% MeOH/CHCl3 as eluant to yield the title compound as a colourless oil (0.035g; 17%) which was converted to the oxalate salt, mp 101°-103° C.

出典