1-(4-溴苯基)-2-甲基丙-1-酮

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

实验步骤: Using an analogous procedure to that described in Example 62, part (i), but starting from 1-bromo-4-(2-methylpropanoyl)benzene and 1,3-propanediol there was thus obtained (in 42% yield) 2-(4-bromophenyl)-2-isopropyl-1,3-dioxane (4.25g), b.p. 116° C. at 0.4 mm Hg; 1H NMR (acid free CDCl3): 0.8 (d, 3 H), 1.15-1.25 (m, 1 H), 1.85 (m, 2 H), 2.0-2.1 (m, 1 H), 3.68 (d of t, 2 H), 3.75-3.85 (m, 2 H) 7.15-7.25 (m, 2 H), 7.45-7.55 (m, 2 H): mass spectrum (CI+) 285 (M+H)+.

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

实验步骤: 4-Bromobenzonitrile (10 g) was dissolved in anhydrous diethyl ether (125 ml) and 2M isopropyl magnesium chloride in diethyl ether (30.24 ml) was added dropwise with stirring. The resulting solution was then heated to reflux for 18 hours. The reaction mixture was allowed to cool to ambient temperature and a saturated aqueous solution of ammonium chloride was added slowly with stirring. Stirring was continued for a further 2 hours. The organic phase was separated and the aqueous layer was extracted with diethyl ether (3×100 ml). The combined organic phases were washed with water (50 ml), then brine (50 ml), dried (MgSO4) and evaporated to give 1-bromo-4-(2-methylpropanoyl)benzene (11.6 g); 1H NMR (CDCl3): 1.15 (d, 6 H), 3.1 (septet, 1 H), 7.5-7.6 (m, 4 H); mass spectrum (CI+) 226 (M.)+. The resulting solution was then heated to reflux for 18 hours with stirring Stirring The organic phase was separated the aqueous layer was extracted with diethyl ether (3×100 ml) The combined organic phases were washed with water (50 ml) brine (50 ml), dried (MgSO4) evaporated

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

实验步骤: Using an analogous procedure to that described in Example 62, part (i), but starting from 1-bromo-4-(2-methylpropanoyl)benzene and 1,3-propanediol there was thus obtained (in 42% yield) 2-(4-bromophenyl)-2-isopropyl-1,3-dioxane (4.25 g), b.p. 116° C. at 0.4 mm Hg 1H NMR (acid free CDCl3): 0.8 (d, 3H), 1.15-1.25 (m, 1H), 1.85 (m, 2H), 2.0-2.1 (m, 1H), 3.68 (d of t, 2H), 3.75-3.85 (m, 2H) 7.15-7.25 (m, 2H), 7.45-7.55 (m, 2H): mass spectrum (CI+) 285 (M+H)+.

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

实验步骤: 4-Bromobenzonitrile (10 g) was dissolved in anhydrous diethyl ether (125 ml) and 2M isopropyl magnesium chloride in diethyl ether (30.24 ml) was added dropwise with stirring. The resulting solution was then heated to reflux for 18 hours. The reaction mixture was allowed to cool to ambient temperature and a saturated aqueous solution of ammonium chloride was added slowly with stirring. Stirring was continued for a further 2 hours. The organic phase was separated and the aqueous layer was extracted with diethyl ether (3×100 ml). The combined organic phases were washed with water (50 ml), then brine (50 ml), dried (MgSO4) and evaporated to give 1-bromo-4-(2-methylpropanoyl)benzene (11.6 g); 1H NMR (CDCl3): 1.15 (d, 6H), 3.1 (septet, 1H), 7.5-7.6 (m, 4H); mass spectrum (CI+) 226 (M.)+. The resulting solution was then heated to reflux for 18 hours with stirring Stirring The organic phase was separated the aqueous layer was extracted with diethyl ether (3×100 ml) The combined organic phases were washed with water (50 ml) brine (50 ml), dried (MgSO4) evaporated

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

实验步骤: Using an analogous procedure to that described in Example 62, part (i), but starting from 1-bromo-4-(2-methylpropanoyl)benzene and 1,3-propanediol there was thus obtained (in 42% yield) 2-(4-bromophenyl)-2-isopropyl-1,3-dioxane (4.25g), b.p. 116° C. at 0.4 mm Hg; 1H NMR (acid free CDCl3): 0.8 (d, 3 H), 1.15-1.25 (m, 1 H), 1.85 (m, 2 H), 2.0-2.1 (m, 1 H), 3.68 (d of t, 2 H), 3.75-3.85 (m, 2 H) 7.15-7.25 (m, 2 H), 7.45-7.55 (m, 2 H): mass spectrum (CI+) 285 (M+H)+.

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

实验步骤: Using an analogous procedure to that described in Example 62, part (i), but starting from 1-bromo-4-(2-methylpropanoyl)benzene and 1,3-propanediol there was thus obtained (in 42% yield) 2-(4-bromophenyl)-2-isopropyl-1,3-dioxane (4.25g), b.p. 116° C. at 0.4 mm Hg; 1H NMR (acid free CDCl3): 0.8 (d, 3 H), 1.15-1.25 (m, 1 H), 1.85 (m, 2 H), 2.0-2.1 (m, 1 H), 3.68 (d of t, 2 H), 3.75-3.85 (m, 2 H) 7.15-7.25 (m, 2 H), 7.45-7.55 (m, 2 H): mass spectrum (CI+) 285 (M+H)+.

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

实验步骤: 4-Bromobenzonitrile (10 g) was dissolved in anhydrous diethyl ether (125 ml) and 2M isopropyl magnesium chloride in diethyl ether (30.24 ml) was added dropwise with stirring. The resulting solution was then heated to reflux for 18 hours. The reaction mixture was allowed to cool to ambient temperature and a saturated aqueous solution of ammonium chloride was added slowly with stirring. Stirring was continued for a further 2 hours. The organic phase was separated and the aqueous layer was extracted with diethyl ether (3×100 ml). The combined organic phases were washed with water (50 ml), then brine (50 ml), dried (MgSO4) and evaporated to give 1-bromo-4-(2-methylpropanoyl)benzene (11.6 g); 1H NMR (CDCl3): 1.15 (d, 6 H), 3.1 (septet, 1 H), 7.5-7.6 (m, 4 H); mass spectrum (CI+) 226 (M.)+. The resulting solution was then heated to reflux for 18 hours with stirring Stirring The organic phase was separated the aqueous layer was extracted with diethyl ether (3×100 ml) The combined organic phases were washed with water (50 ml) brine (50 ml), dried (MgSO4) evaporated

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

实验步骤: Using an analogous procedure to that described in Example 62, part (i), but starting from 1-bromo-4-(2-methylpropanoyl)benzene and 1,3-propanediol there was thus obtained (in 42% yield) 2-(4-bromophenyl)-2-isopropyl-1,3-dioxane (4.25 g), b.p. 116° C. at 0.4 mm Hg; 1H NMR (acid free CDCl3): 0.8 (d, 3H), 1.15-1.25 (m, 1H), 1.85 (m, 2H), 2.0-2.1 (m, 1H), 3.68 (d of t, 2H), 3.75-3.85 (m, 2H) 7.15-7.25 (m, 2H), 7.45-7.55 (m, 2H): mass spectrum (CI+) 285 (M+H)+.

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

实验步骤: 4-Bromobenzonitrile (10 g) was dissolved in anhydrous diethyl ether (125 ml) and 2M isopropyl magnesium chloride in diethyl ether (30.24 ml) was added dropwise with stirring. The resulting solution was then heated to reflux for 18 hours. The reaction mixture was allowed to cool to ambient temperature and a saturated aqueous solution of ammonium chloride was added slowly with stirring. Stirring was continued for a further 2 hours. The organic phase was separated and the aqueous layer was extracted with diethyl ether (3×100 ml). The combined organic phases were washed with water (50 ml), then brine (50 ml), dried (MgSO4) and evaporated to give 1-bromo-4-(2-methylpropanoyl)benzene (11.6 g); 1H NMR (CDCl3): 1.15 (d, 6H), 3.1 (septet, 1H), 7.5-7.6 (m, 4H); mass spectrum (Cl+) 226 (M.)+. The resulting solution was then heated to reflux for 18 hours with stirring Stirring The organic phase was separated the aqueous layer was extracted with diethyl ether (3×100 ml) The combined organic phases were washed with water (50 ml) brine (50 ml), dried (MgSO4) evaporated

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

实验步骤: Using an analogous procedure to that described in Example 62, part (i), but starting from 1-bromo-4-(2-methylpropanoyl)benzene and 1,3-propanediol there was thus obtained (in 42% yield) 2-(4-bromophenyl)-2-isopropyl-1,3-dioxane (4.25 g), b.p. 116° C. at 0.4 mm Hg 1H NMR (acid free CDCl3): 0.8 (d, 3H), 1.15-1.25 (m, 1H), 1.85 (m, 2H), 2.0-2.1 (m, 1H), 3.68 (d of t, 2H), 3.75-3.85 (m, 2H) 7.15-7.25 (m, 2H), 7.45-7.55 (m, 2H): mass spectrum (CI+) 285 (M+H)+.

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

实验步骤: 4-Bromobenzonitrile (10 g) was dissolved in anhydrous diethyl ether (125 ml) and 2M isopropyl magnesium chloride in diethyl ether (30.24 ml) was added dropwise with stirring. The resulting solution was then heated to reflux for 18 hours. The reaction mixture was allowed to cool to ambient temperature and a saturated aqueous solution of ammonium chloride was added slowly with stirring. Stirring was continued for a further 2 hours. The organic phase was separated and the aqueous layer was extracted with diethyl ether (3×100 ml). The combined organic phases were washed with water (50 ml), then brine (50 ml), dried (MgSO4) and evaporated to give 1-bromo-4-(2-methylpropanoyl)benzene (11.6 g); 1H NMR (CDCl3): 1.15 (d, 6H), 3.1 (septet, 1H), 7.5-7.6 (m, 4H); mass spectrum (CI+) 226 (M.)+. The resulting solution was then heated to reflux for 18 hours with stirring Stirring The organic phase was separated the aqueous layer was extracted with diethyl ether (3×100 ml) The combined organic phases were washed with water (50 ml) brine (50 ml), dried (MgSO4) evaporated

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

实验步骤: Using an analogous procedure to that described in Example 62, part (i), but starting from 1-bromo-4-(2-methylpropanoyl)benzene and 1,3-propanediol there was thus obtained (in 42% yield) 2-(4-bromophenyl)-2-isopropyl-1,3-dioxane (4.25g), b.p. 116° C. at 0.4 mm Hg; 1H NMR (acid free CDCl3): 0.8 (d, 3 H), 1.15-1.25 (m, 1 H), 1.85 (m, 2 H), 2.0-2.1 (m, 1 H), 3.68 (d of t, 2 H), 3.75-3.85 (m, 2 H) 7.15-7.25 (m, 2 H), 7.45-7.55 (m, 2 H): mass spectrum (CI+) 285 (M+H)+.