4-propan-2-yloxy-3-(trifluoromethyl)aniline

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

実験手順: A mixture of 54.8 g of 2B and 200 ml of 98% formic acid was refluxed for one hour, cooled and poured into ice water. The resulting mixture was extracted with ether. The extract was washed, successively, with aqueous soidum bicarbonate and water, dried and the solvent was evaporated under reduced pressure. The residue, a syrup, crystallized from 1/5 v/v ether/hexane to give N-(4-isopropoxy-3-(trifluoromethyl)phenyl)formamide (2C), as a tan solid, mp: 80°-82° C. was refluxed for one hour cooled The resulting mixture was extracted with ether The extract was washed successively, with aqueous soidum bicarbonate and water, dried the solvent was evaporated under reduced pressure The residue, a syrup, crystallized from 1/5 v/v ether/hexane

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

実験手順: 137.5 g of iron filings were added in portions to a refluxing mixture of 113.3 g of 2A, 1200 ml of 5% aqueous acetic acid and 50 ml of methanol. The resulting mixture was refluxed for one hour and filtered while hot. Work-up by either extraction of the cooled filtrate gave 4-isopropoxy-3-(trifluoromethyl)aniline (2B), as an amber oil. The resulting mixture was refluxed for one hour filtered while hot Work-up by either extraction of the cooled filtrate

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

実験手順: A mixture of 54.8 g of 2B and 200 ml of 98% formic acid was refluxed for one hour, cooled and poured into ice water. The resulting mixture was extracted with ether. The extract was washed, successively, with aqueous soidum bicarbonate and water, dried and the solvent was evaporated under reduced pressure. The residue, a syrup, crystallized from 1/5 v/v ether/hexane to give N-(4-isopropoxy-3-(trifluoromethyl)phenyl)formamide (2C), as a tan solid, mp: 80°-82° C. was refluxed for one hour cooled The resulting mixture was extracted with ether The extract was washed successively, with aqueous soidum bicarbonate and water, dried the solvent was evaporated under reduced pressure The residue, a syrup, crystallized from 1/5 v/v ether/hexane

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

実験手順: 137.5 g of iron filings were added in portions to a refluxing mixture of 113.3 g of 2A, 1200 ml of 5% aqueous acetic acid and 50 ml of methanol. The resulting mixture was refluxed for one hour and filtered while hot. Work-up by either extraction of the cooled filtrate gave 4-isopropoxy-3-(trifluoromethyl)aniline (2B), as an amber oil. The resulting mixture was refluxed for one hour filtered while hot Work-up by either extraction of the cooled filtrate

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

実験手順: A mixture of 54.8 g of 2B and 200 ml of 98% formic acid was refluxed for one hour, cooled and poured into ice water. The resulting mixture was extracted with ether. The extract was washed, successively, with aqueous soidum bicarbonate and water, dried and the solvent was evaporated under reduced pressure. The residue, a syrup, crystallized from 1/5 v/v ether/hexane to give N-(4-isopropoxy-3-(trifluoromethyl)phenyl)formamide (2C), as a tan solid, mp: 80°-82° C. was refluxed for one hour cooled The resulting mixture was extracted with ether The extract was washed successively, with aqueous soidum bicarbonate and water, dried the solvent was evaporated under reduced pressure The residue, a syrup, crystallized from 1/5 v/v ether/hexane

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

実験手順: 137.5 g of iron filings were added in portions to a refluxing mixture of 113.3 g of 2A, 1200 ml of 5% aqueous acetic acid and 50 ml of methanol. The resulting mixture was refluxed for one hour and filtered while hot. Work-up by either extraction of the cooled filtrate gave 4-isopropoxy-3-(trifluoromethyl)aniline (2B), as an amber oil. The resulting mixture was refluxed for one hour filtered while hot Work-up by either extraction of the cooled filtrate