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ChemicalBook CAS DataBase List 9-Azabicyclo(3.3.1)nonan-3-one Hydrochloride

9-Azabicyclo(3.3.1)nonan-3-one Hydrochloride synthesis

2synthesis methods
-

Yield:72761-60-5 68%

Reaction Conditions:

Stage #1: pseudopelletierinewith carbonochloridic acid 1-chloro-ethyl ester in toluene at 20 - 90; for 44 h;
Stage #2: with methanol for 2 h;Reflux;

Steps:

A

1 -Chloroethylchloroformate (21.4 g, 150 mmol) was added to a mixture of 9- methyl-9-aza-bicyclo[3.3.1]nonan-3-one (15.3 g, 100 mmol) and toluene (100 ml) and was allowed to stir at room-temperature for 15 h. The mixture was stirred at 90°C for 9 h. Another portion of 1 -chloroethylchloroformate (14.3 g, 100 mmol) was added followed by stirring at 90°C for 20 h. Methanol (80 ml) was added fol- lowed by reflux for 2 h. The mixture was cooled on an ice-bath. The pure product precipitated, was filtered and washed with diethylether. Yield 12.0 g (68%).

References:

WO2009/98209,2009,A1 Location in patent:Page/Page column 16

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