(2,3-二甲基苯基)-苯基甲酮

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

实验步骤: The dimethylbenzophenone fraction is contaminated with a small amount (0.05-0.1 lb/lb dimethylbenzophenones) of benzoic acid that co-distills with it. The benzoic acid is removed from the final product as described in Example 1. The washed dimethylbenzophenone product may or may not be given a final distillation in a 10 trays Oldershaw column to improve product color and purity as described in Example 1. Synthesis of dimethylbenzophenone from an isomeric mixture of xylenes will produce a mixture of six dimethylbenzophenone isomers. Synthesis from pure p-xylene will produce only 2,5-dimethylbenzophenone; pure m-xylene will produce 2,4-, 2,5-, and 2,6-dimethylbenzophenone; and pure o-xylene will produce 2,3- and 3,4-dibenzophenone. One can therefore tailor the specific isomeric mixture produced by a provident choice of the composition of the initial xylene mixture. The benzoic acid is removed from the final product distillation in a 10 trays Oldershaw column Synthesis of dimethylbenzophenone will produce

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

实验步骤: The dimethylbenzophenone fraction is contaminated with a small amount (0.05-0.1 lb/lb dimethylbenzophenones) of benzoic acid that co-distills with it. The benzoic acid is removed from the final product as described in Example 1. The washed dimethylbenzophenone product may or may not be given a final distillation in a 10 trays Oldershaw column to improve product color and purity as described in Example 1. Synthesis of dimethylbenzophenone from an isomeric mixture of xylenes will produce a mixture of six dimethylbenzophenone isomers. Synthesis from pure p-xylene will produce only 2,5-dimethylbenzophenone; pure m-xylene will produce 2,4-, 2,5-, and 2,6-dimethylbenzophenone; and pure o-xylene will produce 2,3- and 3,4-dibenzophenone. One can therefore tailor the specific isomeric mixture produced by a provident choice of the composition of the initial xylene mixture. The benzoic acid is removed from the final product distillation in a 10 trays Oldershaw column Synthesis of dimethylbenzophenone will produce

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

实验步骤: To a stirred solution of 2,3-dimethylbenzoyl chloride (35 g, 208 mmol) at 0° in dry dichloroethane (80 ml) was added anhydrous aluminium chloride (27.7 g, 208 mmol) portionwise over two minutes. The mixture was stirred for fifteen minutes and dry benzene (40 ml) was added. After warming to room temperature over fifteen minutes, the mixture was heated to reflux for four hours. The dark solution was cooled, poured onto ice (200 ml) containing concentrated hydrochloric acid (20 ml) and extracted with ether (3×100 ml). The combined organic layers were washed with 10% sodium hydroxide (2×50 ml), 10% sodium carbonate (50 ml) and brine (50 ml). After drying the organic layer over sodium sulphate, the solvent was removed under reduced pressure and the red oil (36 g) so obtained was chromatographed (SiO2 (400 g) using petroleum ether (60°-80°) and chloroform (0-12%) as eluent). This gave the desired 1-benzoyl-2,3 -dimethylbenzene (18.2 g, 42%). the mixture was heated to reflux for four hours The dark solution was cooled poured onto ice (200 ml) extracted with ether (3×100 ml) The combined organic layers were washed with 10% sodium hydroxide (2×50 ml), 10% sodium carbonate (50 ml) and brine (50 ml) After drying the organic layer over sodium sulphate the solvent was removed under reduced pressure

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

实验步骤: The dimethylbenzophenone fraction is contaminated with a small amount (0.05-0.1 lb/lb dimethylbenzophenones) of benzoic acid that co-distills with it. The benzoic acid is removed from the final product as described in Example 1. The washed dimethylbenzophenone product may or may not be given a final distillation in a 10 trays Oldershaw column to improve product color and purity as described in Example 1. Synthesis of dimethylbenzophenone from an isomeric mixture of xylenes will produce a mixture of six dimethylbenzo-phenone isomers. Synthesis from pure p-xylene will produce only 2,5-dimethylbenzophenone; pure m-xylene will produce 2,4-, 2,5-, and 2,6-dimethylbenzophenone; and pure o-xylene will produce 2,3- and 3,4-dimethylbenzophenone. Specific isomeric mixtures are produced by a provident choice of the composition of the initial xylene mixture. The benzoic acid is removed from the final product distillation in a 10 trays Oldershaw column Synthesis of dimethylbenzophenone will produce

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

实验步骤: The dimethylbenzophenone fraction is contaminated with a small amount (0.05-0.1 lb/lb dimethylbenzophenones) of benzoic acid that co-distills with it. The benzoic acid is removed from the final product as described in Example 1. The washed dimethylbenzophenone product may or may not be given a final distillation in a 10 trays Oldershaw column to improve product color and purity as described in Example 1. Synthesis of dimethylbenzophenone from an isomeric mixture of xylenes will produce a mixture of six dimethylbenzo-phenone isomers. Synthesis from pure p-xylene will produce only 2,5-dimethylbenzophenone; pure m-xylene will produce 2,4-, 2,5-, and 2,6-dimethylbenzophenone; and pure o-xylene will produce 2,3- and 3,4-dimethylbenzophenone. Specific isomeric mixtures are produced by a provident choice of the composition of the initial xylene mixture. The benzoic acid is removed from the final product distillation in a 10 trays Oldershaw column Synthesis of dimethylbenzophenone will produce

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

实验步骤: The dimethylbenzophenone fraction is contaminated with a small amount (0.05-0.1 lb/lb dimethylbenzophenones) of benzoic acid that co-distills with it. The benzoic acid is removed from the final product as described in Example 1. The washed dimethylbenzophenone product may or may not be given a final distillation in a 10 trays Oldershaw column to improve product color and purity as described in Example 1. Synthesis of dimethylbenzophenone from an isomeric mixture of xylenes will produce a mixture of six dimethylbenzo-phenone isomers. Synthesis from pure p-xylene will produce only 2,5-dimethylbenzophenone; pure m-xylene will produce 2,4-, 2,5-, and 2,6-dimethylbenzophenone; and pure o-xylene will produce 2,3- and 3,4-dimethylbenzophenone. Specific isomeric mixtures are produced by a provident choice of the composition of the initial xylene mixture. The benzoic acid is removed from the final product distillation in a 10 trays Oldershaw column Synthesis of dimethylbenzophenone will produce

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

实验步骤: The dimethylbenzophenone fraction is contaminated with a small amount (0.05-0.1 lb/lb dimethylbenzophenones) of benzoic acid that co-distills with it. The benzoic acid is removed from the final product as described in Example 1. The washed dimethylbenzophenone product may or may not be given a final distillation in a 10 trays Oldershaw column to improve product color and purity as described in Example 1. Synthesis of dimethylbenzophenone from an isomeric mixture of xylenes will produce a mixture of six dimethylbenzophenone isomers. Synthesis from pure p-xylene will produce only 2,5-dimethylbenzophenone; pure m-xylene will produce 2,4-, 2,5-, and 2,6-dimethylbenzophenone; and pure o-xylene will produce 2,3- and 3,4-dibenzophenone. One can therefore tailor the specific isomeric mixture produced by a provident choice of the composition of the initial xylene mixture. The benzoic acid is removed from the final product distillation in a 10 trays Oldershaw column Synthesis of dimethylbenzophenone will produce

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

实验步骤: To a stirred solution of 2,3-dimethylbenzoyl chloride (35 g, 208 mmol) at 0° in dry dichloroethane (80 ml) was added anhydrous aluminium chloride (27.7 g, 208 mmol) portionwise over two minutes. The mixture was stirred for fifteen minutes and dry benzene (40 ml) was added. After warming to room temperature over fifteen minutes, the mixture was heated to reflux for four hours. The dark solution was cooled, poured onto ice (200 ml) containing concentrated hydrochloric acid (20 ml) and extracted with ether (3×100 ml). The combined organic layers were washed with 10% sodium hydroxide (2×50 ml), 10% sodium carbonate (50 ml) and brine (50 ml). After drying the organic layer over sodium sulphate, the solvent was removed under reduced pressure and the red oil (36 g) so obtained was chromatographed (SiO2 (400 g) using petroleum ether (60°-80°) and chloroform (0-12%) as eluent). This gave the desired 1-benzoyl-2,3 -dimethylbenzene (18.2 g, 42%). the mixture was heated to reflux for four hours The dark solution was cooled poured onto ice (200 ml) extracted with ether (3×100 ml) The combined organic layers were washed with 10% sodium hydroxide (2×50 ml), 10% sodium carbonate (50 ml) and brine (50 ml) After drying the organic layer over sodium sulphate the solvent was removed under reduced pressure