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ChemicalBook CAS DataBase List 2,3,4,5-Tetrahydro-3-(trifluoroacetyl)-1,5-methano-1H-3-benzazepine
230615-51-7

2,3,4,5-Tetrahydro-3-(trifluoroacetyl)-1,5-methano-1H-3-benzazepine synthesis

3synthesis methods
-

Yield:-

Reaction Conditions:

with triethylamine in dichloromethane at 0 - 20;Product distribution / selectivity;

Steps:

8
A suspension of 10-Aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-triene hydrochloride (500 g) and MDC (8 l) was stirred at 0° to 5° C., and treated with triethylamine (621.4 g). To this solution, tri-fluoro acetic anhydride (645 g) was added at 0° to 5° C. over 30 to 40 minutes. The resulting solution was allowed to warm to room temperature, and stirred for 2 hours. The progress of the reaction was checked by HPLC. The reaction was quenched by addition of DM water (3.75 l) at 5° to 10° C., and stirred for 1.0 hour. The layers were separated, and the aqueous layer was extracted with MDC (1 l). The organic layer was washed with 1N HCl (3×3 l) and 10 percent aqueous sodium chloride solution (2 l). Concentration of the organic layer to 2 l provided a 1-(10-Aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-triene-10-yl)-2,2,2-trifluoro ethenone product, which was further processed as described below stage (HPLC purity 98.12 percent).

References:

Kansal, Vinod Kumar;Ahmad, Suhail;Gupta, Amit US2009/318695, 2009, A1 Location in patent:Page/Page column 9

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