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D. 3,4-Diamino-6-fluorobenzotrifluoride A mixture of 3-amino-6-fluoro-4-nitrobenzotrifluoride (328 mg, 1.45 mmol) and 10% Pd/C (50 mg) in ethanol (15 mL) was hydrogenated for 2 h at 25 C. under 25 psi H2. The catalyst was removed by filtration with celite and the solvent was removed by rota-evaporation to give 270 mg of 3,4-diamino-6-fluorobenzotrifluoride (95%) as a brown solid. 1 H NMR (CDCl3): delta3.432 (br, 4H), 6.469 (d, 1H, J=8.4 Hz); 6.860 (d, 1H, J=6.6 Hz).
With tin(ll) chloride; In ethanol; at 65 - 70℃;
To a stirred solution of 11.35 g (50.6 mmol) of the nitroaniline 18a in 250 mL of ethanol was added 57.1 g (253 mmol) of tin (II) chloride dihydrate at room temperature. The reaction was heated at 65-70 C. for 45 minutes. The reaction was cooled and poured into 900 mL of ice water. It was basified to pH 8 with solid sodium bicarbonate and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, and evaporated to give 9.33 g of compound 19a as a dark red solid. Calcd for C7H6F4N4.H+=195; Found m/z=195.
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