benzyl thiocyanate

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:

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

実験手順: A solution of 5-bromo-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulphonylpyrazole (3.0 g) in dry tetrahydrcfuran (32 ml , stirred under nitrogen at -78° C., was treated with a solution of n-butyllithium in hexane (2.8 ml of a 2.5M solution) over a period of 5 minutes. After 1 hour at -78° C., a solution of benzyl thiocyanate (0.95 g) in tetrahydrofuran (2 ml) was added. The stirred mixture was allowed to warm slowly to room temperature during 16 hours, then poured onto ice/water 50 ml) and extracted with ether (3×50 ml). The combined extracts were dried over anhydrous magnesium sulphate, evaporated in vacuo, and purified by chromatography, eluting with ethyl acetate/hexane (2:98). The product was triturated with hexane to give 5-benzylthio-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulphonylpyrazole (0.25 g), as a white solid, m.p. 117°-119° C. poured onto ice/water 50 ml) and extracted with ether (3×50 ml) The combined extracts were dried over anhydrous magnesium sulphate evaporated in vacuo purified by chromatography eluting with ethyl acetate/hexane (2:98) The product was triturated with hexane

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Benzyl thiocyanate (29.8 g, 0.2 mol), chloroform (76 g, 0.6 mol) and triethylbenzylammonium chloride (0.5 g, 0.002 mol) were stirred vigorously. 40 ml of 50% aqueous sodium hydroxide were added clowly to this solution (mildly exothermic). The temperature increased to 40° C. and was maintained thereat for 4 h with efficient stirring. was maintained

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Benzyl thiocyanate (29.8 g, 0.2 mol), chloroform (76 g, 0.6 mol) and triethylbenzylammonium chloride (0.5 g, 0.002 mol) were stirred vigorously. 40 ml of 50% aqueous sodium hydroxide were added clowly to this solution (mildly exothermic). The temperature increased to 40° C. and was maintained thereat for 4 h with efficient stirring. was maintained

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 5-bromo-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulphonylpyrazole (3.0 g) in dry tetrahydrofuran (32 ml), stirred under nitrogen at -78° C., was treated with a solution of n-butyllithium in hexane (2.8 ml of a 2.5M solution) over a period of 5 minutes. After 1 hour at -78° C., a solution of benzyl thiocyanate (0.95 g) in tetrahydrofuran (2 ml) was added. The stirred mixture was allowed to warm slowly to room temperature during 16 hours, then poured onto ice/water (50 ml) and extracted with ether (3×50 ml). The combined extracts were dried over anhydrous magnesium sulphate, evaporated in vacuo, and purified by chromatography, eluting with ethyl acetate/hexane (2:98). The product was triturated with hexane to give 5-benzylthio-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulphonylpyrazole (0.25 g), as a white solid, m.p. 117°-119° C. poured onto ice/water (50 ml) extracted with ether (3×50 ml) The combined extracts were dried over anhydrous magnesium sulphate evaporated in vacuo purified by chromatography eluting with ethyl acetate/hexane (2:98) The product was triturated with hexane

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

実験手順: A solution of 5-bromo-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulphonylpyrazole (3.0 g) in dry tetrahydrcfuran (32 ml , stirred under nitrogen at -78° C., was treated with a solution of n-butyllithium in hexane (2.8 ml of a 2.5M solution) over a period of 5 minutes. After 1 hour at -78° C., a solution of benzyl thiocyanate (0.95 g) in tetrahydrofuran (2 ml) was added. The stirred mixture was allowed to warm slowly to room temperature during 16 hours, then poured onto ice/water 50 ml) and extracted with ether (3×50 ml). The combined extracts were dried over anhydrous magnesium sulphate, evaporated in vacuo, and purified by chromatography, eluting with ethyl acetate/hexane (2:98). The product was triturated with hexane to give 5-benzylthio-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulphonylpyrazole (0.25 g), as a white solid, m.p. 117°-119° C. poured onto ice/water 50 ml) and extracted with ether (3×50 ml) The combined extracts were dried over anhydrous magnesium sulphate evaporated in vacuo purified by chromatography eluting with ethyl acetate/hexane (2:98) The product was triturated with hexane

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Benzyl thiocyanate (29.8 g, 0.2 mol), chloroform (76 g, 0.6 mol) and triethylbenzylammonium chloride (0.5 g, 0.002 mol) were stirred vigorously. 40 ml of 50% aqueous sodium hydroxide were added slowly to this solution (mildly exothermic). The temperature increased to 40° C. and was maintained thereat for 4 h with efficient stirring. was maintained

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Benzyl thiocyanate (29.8 g, 0.2 mol), chloroform (76 g, 0.6 mol) and triethylbenzylammonium chloride (0.5 g, 0.002 mol) were stirred vigorously. 40 ml of 50% aqueous sodium hydroxide were added clowly to this solution (mildly exothermic). The temperature increased to 40° C. and was maintained thereat for 4 h with efficient stirring. was maintained