Reaktion #1783066

Reaktionsgleichung

EtOAc

tert-butyl 4-(2-nitrobenzylamino)piperidine-1-carboxylate

CDI

DCM

→

solid

Ausbeute 24.4%

tert-Butyl 4-(1,2-dihydro-2-oxoquinazolin-3(4H)-yl)piperidine-1-carboxylate

Ausbeute 24.4%

Lösungsmittel

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture was evaporated
2. 2
   Sonstigeto give an oil that, when
3. 3
   Sonstigeprecipitated the desired product
4. 4
   WaschenThe precipitate was washed with cold EtOAc
5. 5
   Sonstigedried

Vorschrift

To a solution of tert-butyl 4-(2-nitrobenzylamino)piperidine-1-carboxylate (13.2 g, 43.2 mmol) in THF (400 ml) was added a solution of CDI (7.7 g, 47.5 mmol) in 1:1 DCM:THF (100 ml) dropwise over 1 hour followed by stirring the reaction mixture for a further 16 hours. The reaction mixture was evaporated to give an oil that, when treated with EtOAc, precipitated the desired product. The precipitate was washed with cold EtOAc and dried to give a yellow solid (3.5 g). LC/MS (10% to 99%): M/Z (M+H)+ (obs)=332; tR=3.01.

Quelle