Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

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

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

2,3,4,5-Tetrahydro-3-(trifluoroacetyl)-1,5-methano-1H-3-benzazepine Related Search: