2-tert-butyl-2-[2-(4-chlorophenyl)ethyl]oxirane

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 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol was heated in a bomb tube at 150° C. for 20 hours. The reaction solution was allowed to cool and was concentrated. The residue was dissolved in ether and the solution was washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentane-3-ol were obtained as a viscous oil. to cool was concentrated The residue was dissolved in ether the solution was washed three times with water once with sodium chloride solution, dried over sodium sulphate concentrated The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1)

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

実験手順: A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol was heated in a bomb tube at 150° C. for 20 hours. The reaction solution was allowed to cool and was concentrated. The residue was dissolved in ether and the solution was washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentane-3-ol were obtained as a viscous oil. to cool was concentrated The residue was dissolved in ether the solution was washed three times with water once with sodium chloride solution, dried over sodium sulphate concentrated The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1)

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

実験手順: A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol was heated in a bomb tube at 150° C. for 20 hours. The reaction solution was allowed to cool and was concentrated. The residue was dissolved in ether and the solution was washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentane-3-ol were obtained as a viscous oil. to cool was concentrated The residue was dissolved in ether the solution was washed three times with water once with sodium chloride solution, dried over sodium sulphate concentrated The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1)

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 17 9 g (0.075 mol) of 2-(4-chloro-phenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mol) of 1,2,4-triazole in 30 ml of ethanol is heated at 150° C. in a bomb tube for 20 hours. The reaction solution is allowed to cool and is concentrated. The residue is dissolved in ether and the solution is washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue is chromatographed over a silica gel column (running agent: methylene chloride/ethyl acetate=1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentan-3-ol obtained as a viscous oil, which can be recrystallized from acetonitrile (melting point 102° to 104° C.). to cool is concentrated The residue is dissolved in ether the solution is washed three times with water once with sodium chloride solution, dried over sodium sulphate concentrated The residue is chromatographed over a silica gel column (running agent: methylene chloride/ethyl acetate=1:1)

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

実験手順: A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyloxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol in a sealed tube is heated at 150° C. for 20 hours. The tube is allowed to cool and the reaction solution is evaporated. The residue is dissolved in ether, washed three times with water and once with sodium chloride solution, dried over sodium sulphate and evaporated. The residue is chromatographed over a column of silican gel (mobile phase: dichloroethane/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-3-pentanol are obtained as a viscous oil. to cool the reaction solution is evaporated The residue is dissolved in ether washed three times with water once with sodium chloride solution, dried over sodium sulphate evaporated The residue is chromatographed over a column of silican gel (mobile phase: dichloroethane/ethyl acetate 1:1)

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

実験手順: A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyloxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol in a sealed tube is heated at 150° C. for 20 hours. The tube is allowed to cool and the reaction solution is evaporated. The residue is dissolved in ether, washed three times with water and once with sodium chloride solution, dried over sodium sulphate and evaporated. The residue is chromatographed over a column of silican gel (mobile phase: dichloroethane/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-3-pentanol are obtained as a viscous oil. to cool the reaction solution is evaporated The residue is dissolved in ether washed three times with water once with sodium chloride solution, dried over sodium sulphate evaporated The residue is chromatographed over a column of silican gel (mobile phase: dichloroethane/ethyl acetate 1:1)

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

実験手順: A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol was heated in a bomb tube at 150° C. for 20 hours. The reaction solution was allowed to cool and was concentrated. The residue was dissolved in ether and the solution was washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentane-3-ol were obtained as a viscous oil. to cool was concentrated The residue was dissolved in ether the solution was washed three times with water once with sodium chloride solution, dried over sodium sulphate concentrated The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1)

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

実験手順: A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol was heated in a bomb tube at 150° C. for 20 hours. The reaction solution was allowed to cool and was concentrated. The residue was dissolved in ether and the solution was washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentane-3-ol were obtained as a viscous oil. to cool was concentrated The residue was dissolved in ether the solution was washed three times with water once with sodium chloride solution, dried over sodium sulphate concentrated The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1)

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

実験手順: A solution of 17.9 g (0.075 mole) of 2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane and 6.9 g (0.1 mole) of 1,2,4-triazole in 30 ml of ethanol was heated in a bomb tube at 150° C. for 20 hours. The reaction solution was allowed to cool and was concentrated. The residue was dissolved in ether and the solution was washed three times with water and once with sodium chloride solution, dried over sodium sulphate and concentrated. The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1). 12.3 g (53.2% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentane-3-ol were obtained as a viscous oil. to cool was concentrated The residue was dissolved in ether the solution was washed three times with water once with sodium chloride solution, dried over sodium sulphate concentrated The residue was chromatographed over a silica gel column (mobile phase: methylene chloride/ethyl acetate 1:1)