3,5-二甲基-4-苯基二烯基苯酚

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of sodium (2.0 g) in absolute alcohol (120 ml) was added 2,6-dimethyl-4-hydroxyazobenzene (18.3 g) and 1-bromo propane (20 g). The mixture was refluxed for three hours and was left overnight at room temperature. A precipitate of sodium bromide was filtered off, was washed with some cold absolute ethanol, and was discarded. The alcohol was removed from the filtrate by distillation, the residue was dissolved in ether (200 ml), and was extracted with 2% sodium hydroxide solution (4×50 ml) and once with water. After drying (Na2SO4) and filtering, the ether solution was evaporated to dryness leaving a residual oily material (20.2 g), sufficiently pure for the following reaction step. The mixture was refluxed for three hours A precipitate of sodium bromide was filtered off was washed with some cold absolute ethanol The alcohol was removed from the filtrate by distillation the residue was dissolved in ether (200 ml) was extracted with 2% sodium hydroxide solution (4×50 ml) and once with water After drying (Na2SO4) filtering the ether solution was evaporated to dryness

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of sodium (2.0 g, 0.09 mole) in absolute ethanol (119 ml) was added 2,6-dimethyl-4-hydroxyazobenzene (18.3 g, 0.08 mole) prepared according to B. C. Saunders and G. H. R. Watson, Biochem. J. 46:629-233 (1950). To the resulting orange-red solution was added 1-bromobutane (22.3 g, 0.162 mole) slowly from a separatory funnel and the mixture was refluxed for five hours. When cool, the precipitated sodium bromide was filtered off and the filtrate was evaporated to dryness. The residue was taken up in ether and the ether solution was extracted, first with 0.5 M sodium hydroxide and then once with water. The ether phase was dried (Na2SO4), filtered, and evaporated to dryness. The yield was over 90%. This material is satisfactory for the next step. After recrystallization from 95% ethanol, it melted at 47°-47.5° C. Calcd. for C18H22N2O: C 76.6, H 7.85, N 9.92. Found: C 76.7, H 7.84, N 9.86. prepared the mixture was refluxed for five hours When cool the precipitated sodium bromide was filtered off the filtrate was evaporated to dryness the ether solution was extracted, first with 0.5 M sodium hydroxide The ether phase was dried (Na2SO4) filtered evaporated to dryness After recrystallization from 95% ethanol, it melted at 47°-47.5° C

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of sodium (2.0 g) in absolute alcohol (120 ml) was added 2,6-dimethyl-4-hydroxyazobenzene (18.3 g) and 1-bromo propane (20 g). The mixture was refluxed for three hours and was left overnight at room temperature. A precipitate of sodium bromide was filtered off, was washed with some cold absolute ethanol, and was discarded. The alcohol was removed from the filtrate by distillation, the residue was dissolved in ether (200 ml), and was extracted with 2% sodium hydroxide solution (4×50 ml) and once with water. After drying (Na2SO4) and filtering, the ether solution was evaporated to dryness leaving a residual oily material (20.2 g), sufficiently pure for the following reaction step. The mixture was refluxed for three hours A precipitate of sodium bromide was filtered off was washed with some cold absolute ethanol The alcohol was removed from the filtrate by distillation the residue was dissolved in ether (200 ml) was extracted with 2% sodium hydroxide solution (4×50 ml) and once with water After drying (Na2SO4) filtering the ether solution was evaporated to dryness

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of sodium (2.0 g, 0.09 mole) in absolute ethanol (119 ml) was added 2,6-dimethyl-4-hydroxyazobenzene (18.3 g, 0.08 mole) prepared according to B. C. Saunders and G. H. R. Watson, Biochem. J. 46:629-233 (1950). To the resulting orange-red solution was added 1-bromobutane (22.3 g, 0.162 mole) slowly from a separatory funnel and the mixture was refluxed for five hours. When cool, the precipitated sodium bromide was filtered off and the filtrate was evaporated to dryness. The residue was taken up in ether and the ether solution was extracted, first with 0.5 M sodium hydroxide and then once with water. The ether phase was dried (Na2SO4), filtered, and evaporated to dryness. The yield was over 90%. This material is satisfactory for the next step. After recrystallization from 95% ethanol, it melted at 47°-47.5° C. prepared the mixture was refluxed for five hours When cool the precipitated sodium bromide was filtered off the filtrate was evaporated to dryness the ether solution was extracted, first with 0.5 M sodium hydroxide The ether phase was dried (Na2SO4) filtered evaporated to dryness After recrystallization from 95% ethanol, it melted at 47°-47.5° C.

反应条件: temp:0.00; pressure:0.00; stir: