Stannous Chloride → 7-Fluoro-2-trifluoromethyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride

関与物質

反応手順

Heat a solution of 2-(5-fluoro-2-nitro-phenylamino)-5-trifluoromethyl-benzonitrile (1.62 g, 4.98 mmol) in ethanol (24 ml) to 60° C. Add to this a solution of tin (II) chloride (2.83 g, 14.94 mmol) in 5.0 N hydrochloric acid (24 ml). Heat the resulting mixture to reflux for 20 hours. Cool the reaction to room temperature, add 30 ml of 5.0 N hydrochloric acid and place the mixture in a freezer for 16 hours. The product precipitates from the solution and is collected by filtration. Wash solid with 5.0 N hydrochloric acid to obtain 1.44 g of the title compound (4.34 mmol, 87% yield) as a yellow amorphous solid: Mass Spectrum (m/e): 295(M+1).

情報源と証拠