反応 #332184

反応方程式

Trimethylsilyl cyanide

43a

4-(4-aminophenyl)-piperazine-1-carboxylic acid tert-butyl ester

cyclobutanone

sodium sulfate

→

43b

収率 84.0%

4-[4-(1-cyanocyclobutylamino)phenyl]-piperazine-1-carboxylic acid tert-butyl ester

収率 84.0%

溶媒

dichloromethane

acetone

dichloromethane

反応条件

後処理

1. 1
   ろ過After filtration
2. 2
   濃縮the medium was concentrated under vacuum
3. 3
   その他to obtain a brown liquid which

実験手順

Trimethylsilyl cyanide (0.3 g, 3 mmol) was added dropwise to a mixture of 43a (0.415 g, 1.5 mmol), cyclobutanone (0.21 g, 3 mmol) and sodium sulfate (1 g) in dichloromethane (5 ml). The mixture was stirred for 15 hours. After filtration to eliminate sodium sulfate, the medium was concentrated under vacuum to obtain a brown liquid which was subjected to chromatography (dichloromethane:acetone, 75:25) to yield 43b (0.448 g, 1.26 mmol, 84%) as a yellow solid.

出典