4-amino-3-(trifluoromethyl)phenol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This material is prepared by a method analogous to that described for preparation of 2C, starting from 4-amino-3-(trifluoromethyl) phenol and 4-chloro-2-cyanopyridine. This material is prepared by a method analogous to

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This material is prepared by a method analogous to that described for preparation of 2C, starting from 4-amino-3-(trifluoromethyl)phenol and 4-chloro-2-cyanopyridine. This material is prepared by a method analogous to

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Amino-3-trifluoromethylphenol (0.212 g; 1.2 mmol) was dissolved in 10 ml of glacial acetic acid under nitrogen atmosphere and acetic anhydride (0.3 ml; 3.0 mmol) was added followed with stirring for an hour at room temperature. Water (0.5 ml) was added into the reaction mixture and then evaporated to dryness. Toluene (50 ml) was added and the evaporation was repeated to give a quantitative yield of pure N-(4-Hydroxy-2-trifluoromethylphenyl)acetamide. 1H NMR (400 MHz, DMSO-d6): 1.99 (3H, s), 7.01 (1H, dd, J=8.6 Hz, J=2.6 Hz), 7.02 (1H, d, J=2.5 Hz), 7.19 (1H, d, J=8.4 Hz), 9.33 (1H, s), 10.08 (1H, br s). evaporated to dryness Toluene (50 ml) was added the evaporation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Nitro-3-trifluoromethylphenol (0.414 g; 2.0 mmol) was dissolved in 25 ml of glacial acetic acid and zinc dust (2.62 g; 40 mmol) was added in small portions during 10 minutes allowing the temperature to rise up to +40° C. The mixture was stirred for ten minutes and filtered. The dust was washed with 3×10 ml of glacial acetic acid and filtrate was evaporated to dryness to give 0.212 g of 4-amino-3-trifluoromethylphenol. 1H NMR (400 MHz, DMSO-d6): 4.86 (2H, s), 6.72 (1H, d, J=8.7 Hz), 6.74 (1H, d, J=2.6 Hz), 6.78 (1H, dd, J=8.7 Hz, J=2.7 Hz), 8.91 (1H, s) to rise up to +40° C filtered The dust was washed with 3×10 ml of glacial acetic acid and filtrate was evaporated to dryness

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Amino-3-trifluoromethylphenol (0.212 g; 1.2 mmol) was dissolved in 10 ml of glacial acetic acid under nitrogen atmosphere and acetic anhydride (0.3 ml; 3.0 mmol) was added followed with stirring for an hour at room temperature. Water (0.5 ml) was added into the reaction mixture and then evaporated to dryness. Toluene (50 ml) was added and the evaporation was repeated to give a quantitative yield of pure N-(4-Hydroxy-2-trifluoromethylphenyl)acetamide. 1H NMR (400 MHz, DMSO-d6): 1.99 (3H, s), 7.01 (1H, dd, J=8.6 Hz, J=2.6 Hz), 7.02 (1H, d, J=2.5 Hz), 7.19 (1H, d, J=8.4 Hz), 9.33 (1H, s), 10.08 (1H, br s). evaporated to dryness Toluene (50 ml) was added the evaporation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Nitro-3-trifluoromethylphenol (0.414 g; 2.0 mmol) was dissolved in 25 ml of glacial acetic acid and zinc dust (2.62 g; 40 mmol) was added in small portions during 10 minutes allowing the temperature to rise up to +40° C. The mixture was stirred for ten minutes and filtered. The dust was washed with 3×10 ml of glacial acetic acid and filtrate was evaporated to dryness to give 0.212 g of 4-amino-3-trifluoromethylphenol. 1H NMR (400 MHz, DMSO-d6): 4.86 (2H, s), 6.72 (1H, d, J=8.7 Hz), 6.74 (1H, d, J=2.6 Hz), 6.78 (1H, dd, J=8.7 Hz, J=2.7 Hz), 8.91 (1H, s) to rise up to +40° C filtered The dust was washed with 3×10 ml of glacial acetic acid and filtrate was evaporated to dryness

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 4-nitro-3-(trifluoromethyl)phenol (Aldrich, 414 mg, 2.0 mmol) in 10 mL of MeOH was added 10% Pd/C (100 mg). The suspension was stirred under H2 atmosphere for 12 h and it was then filtered and concentrated in vacuo to give 4-amino-3-(trifluoromethyl)phenol (350 mg, 95% yield), which was sufficiently pure to use in the next step. MS(ESI+): m/z 178.02 (M+H)+. it was then filtered concentrated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: This material is prepared by a method analogous to that described for preparation of 2C, starting from 4-amino-3-(trifluoromethyl) phenol and 4-chloro-2-cyanopyridine. This material is prepared by a method analogous to