3-甲氧基-1-苯基丙-1-one

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of ethyl magnesium bromide in diethyl ether (58 ml, 3 M) was added dropwise at room temperature to a mixture of 3-methoxybenzonitrile (21.2 g, 0.159 mol) and dry THF (250 ml). When addition was complete the mixture was stirred for 1 h at room temperature, 3 h at 40° C. and finally stirred overnight at room temperature. Water (250 ml) was added followed by a saturated ammonium chloride solution (250 ml) and the mixture was stirred for 1 h at room temperature. The phases were separated and the aqueous phase was extracted with ethyl acetate (100 ml). The combined organic phases was dried (MgSO4) and the solvent evaporated in vacuo to give 25.9 g (99%) of 3-methoxypropiophenone. When addition the mixture was stirred for 1 h at room temperature The phases were separated the aqueous phase was extracted with ethyl acetate (100 ml) The combined organic phases was dried (MgSO4) the solvent evaporated in vacuo

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of ethyl magnesium bromide in diethyl ether (58 ml, 3 M) was added dropwise at room temperature to a mixture of 3-methoxybenzonitrile (21.2 g, 0.159 mol) and dry THF (250 ml). When addition was complete the mixture was stirred for 1 h at room temperature, 3 h at 40° C. and finally stirred overnight at room temperature. Water (250 ml) was added followed by a saturated ammonium chloride solution (250 ml) and the mixture was stirred for 1 h at room temperature. The phases were separated and the aqueous phase was extracted with ethyl acetate (100 ml). The combined organic phases was dried (MgSO4) and the solvent evaporated in vacuo to give 25.9 g (99%) of 3-methoxypropiophenone. When addition the mixture was stirred for 1 h at room temperature The phases were separated the aqueous phase was extracted with ethyl acetate (100 ml) The combined organic phases was dried (MgSO4) the solvent evaporated in vacuo

反应条件: temp:-70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-methoxyphenylmagnesium bromide in tetrahydrofuran (500 ml) was prepared from 3-methoxybromobenzene (187 g) and magnesium turnings (24 g) and was added over 1.5 hours to a mixture of propionic anhydride (260 g) and diethyl ether (500 ml) which had been cooled to -70° C. A saturated aqueous solution of ammonium chloride (500 ml) was added and the mixture was allowed to warm to ambient temperature. The organic layer was separated and washed in turn with a dilute aqueous sodium hydroxide solution and with a saturated aqueous sodium chloride solution. The organic layer was dried (Na2SO4) and evaporated to give 3-methoxypropiophenone as a yellow oil (160 g). to warm to ambient temperature The organic layer was separated washed in turn with a dilute aqueous sodium hydroxide solution and with a saturated aqueous sodium chloride solution The organic layer was dried (Na2SO4) evaporated

反应条件: temp:-70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-methoxyphenylmagnesium bromide in tetrahydrofuran (500 ml) was prepared from 3-methoxybromobenzene (187 g) and magnesium turnings (24 g) and was added over 1.5 hours to a mixture of propionic anhydride (260 g) and diethyl ether (500 ml) which had been cooled to -70° C. A saturated aqueous solution of ammonium chloride (500 ml) was added and the mixture was allowed to warm to ambient temperature. The organic layer was separated and washed in turn with a dilute aqueous sodium hydroxide solution and with a saturated aqueous sodium chloride solution. The organic layer was dried (Na2SO4) and evaporated to give 3-methoxypropiophenone as a yellow oil (160 g). to warm to ambient temperature The organic layer was separated washed in turn with a dilute aqueous sodium hydroxide solution and with a saturated aqueous sodium chloride solution The organic layer was dried (Na2SO4) evaporated

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of ethyl magnesium bromide in diethyl ether (58 ml, 3 M) was added dropwise at room temperature to a mixture of 3-methoxybenzonitrile (21.2 g, 0.159 mol) and dry THF (250 ml). When addition was complete the mixture was stirred for 1 h at room temperature, 3 h at 40° C. and finally stirred overnight at room temperature. Water (250 ml) was added followed by a saturated ammonium chloride solution (250 ml) and the mixture was stirred for 1 h at room temperature. The phases were separated and the aqueous phase was extracted with ethyl acetate (100 ml). The combined organic phases was dried (MgSO4) and the solvent evaporated in vacuo to give 25.9 g (99%) of 3-methoxypropiophenone. When addition the mixture was stirred for 1 h at room temperature The phases were separated the aqueous phase was extracted with ethyl acetate (100 ml) The combined organic phases was dried (MgSO4) the solvent evaporated in vacuo