Reaktion #587646

Reaktionsgleichung

HCl

tert-butyl 7-benzyl-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate

N2

→

tert-Butyl 7-benzyl-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate hydrochloride

Lösungsmittel

diethyl ether

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeformed
2. 2
   workup.ADDITIONAfter addition
3. 3
   Filtrationwas collected by filtration
4. 4
   Sonstigedried in a vacuum oven (40° C., 13.3 Pa (0.1 mmHg))

Vorschrift

A solution of tert-butyl 7-benzyl-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate (39.5 g, 0.12 mol) in ethyl acetate (200 mL) was cooled to −10° C. under an inert atmosphere (N2). A solution of HCl in diethyl ether (1 M) was added over the course of 1 h, during which time a precipitate formed. After addition was complete, the resulting mixture was stirred for a further 1 h before the crystalline precipitate was collected by filtration and dried in a vacuum oven (40° C., 13.3 Pa (0.1 mmHg)). This gave 42.6 g (100% from the compound of step (iii) above) of the sub-title compound as an off-white crystalline material.

Quelle