2-nitropropan-1-ol

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:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 36.6 g (0.34 mol) of crude 2-nitro-propan-1-ol [prepared according to Example 1a]in 200 ml of toluene in a pressure vessel is added 2 g of sodium bisulfate [NaHSO4]. Through the closed autoclave is added at room temperature 48 g (0.85 mol) of isobutene. The reaction mixture is maintained at 60° C. for 8 hours. The reaction mixture is cooled to room temperature, diluted with toluene and filtered to give a crude solution of 1-tert-butoxy-2-nitro-propane in toluene. The reaction mixture is cooled to room temperature filtered

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 stirred mixture of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoic acid (50 g, 0.139 mole), 2-nitropropanol (13.2 g, 0.126 mole) and conc. sulfuric acid (1 ml) in benzene (500 ml) was heated to reflux for 24 hours, during which time water (1.9 g) was removed via a Dean Stark trap. The solvent was stripped under reduced pressure and the residue poured into water (700 ml). The product was extracted into ether, which was washed with water and then with 5% sodium bicarbonate. The dried ether solution was concentrated to give 23.2 g of an amber oil which slowly solidified to a tacky semi-solid. was heated was removed via a Dean Stark trap the residue poured into water (700 ml) The product was extracted into ether, which was washed with water The dried ether solution was concentrated

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

実験手順: A stirred mixture of 0.5 g (0.0013 mole) of 2-[2,4-dichloro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]propionic acid (Compound A1), 1.0 g (0.0095 mole) of 2-nitro-1-propanol and 0.05 g (0.0003 mole) of p-toluenesulfonic acid monohydrate in 60 mL of toluene was heated at reflux. The water generated in the reaction was removed by collection in a Dean-Stark trap. After refluxing for a total of two hours, the solvent was removed by distillation under reduced pressure leaving a residue. This residue was dissolved in diethyl ether and washed first with water then with an aqueous 10% sodium hydroxide solution. The organic phase was dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated to yield 0.5 g of 2-nitropropyl 2-[2,4-dichloro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]propionate as an oil, Compound B1. was heated at reflux was removed by collection in a Dean-Stark trap After refluxing for a total of two hours the solvent was removed by distillation under reduced pressure leaving a residue washed first with water The organic phase was dried over anhydrous magnesium sulfate filtered The filtrate was evaporated

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 36.6 g (0.34 mol) of crude 2-nitro-propan-1-ol [prepared according to Example 1a]in 200 ml of toluene in a pressure vessel is added 2 g of sodium bisulfate [NaHSO4]. Through the closed autoclave is added at room temperature 48 g (0.85 mol) of isobutene. The reaction mixture is maintained at 60° C. for 8 hours. The reaction mixture is cooled to room temperature, diluted with toluene and filtered to give a crude solution of 1-tert-butoxy-2-nitro-propane in toluene. The reaction mixture is cooled to room temperature filtered