Reaktion #517056

Reaktionsgleichung

bis(2-chloroethyl)-N-(1,1-dimethylethoxy)carbonyl amine

homophthalonitrile

cesium carbonate

→

4-cyano-N-(1,1-dimethylethoxy)carbonyl-4-(2-cyanophenyl) piperidine

Lösungsmittel

EtOAc

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with saturated aqueous NaHSO4 and saturated aqueous NaCl
2. 2
   TrocknenThe solution was dried over Na2SO4
3. 3
   Einengenconcentrated in vacuo
4. 4
   Sonstigepurified by PCTLC (30% EtOAc in Hexane)

Vorschrift

A solution of bis(2-chloroethyl)-N-(1,1-dimethylethoxy)carbonyl amine (19 g, 78 mmol) and homophthalonitrile (8.6 g, 60 mmol) and cesium carbonate (79 g, 241 mmol) was stirred at 60° C. for 12 hours. The solution cooled to room temperature and diluted with 500 ml EtOAc and washed with saturated aqueous NaHSO4 and saturated aqueous NaCl. The solution was dried over Na2SO4, concentrated in vacuo, and purified by PCTLC (30% EtOAc in Hexane) to afforded 4-cyano-N-(1,1-dimethylethoxy)carbonyl-4-(2-cyanophenyl) piperidine as a yellow/orange oil.

Quelle