1,3,3,3-tetrachloropropylbenzene

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

实验步骤: A mixture of 77.4 g of 1,1,1,3-tetrachloro-3-phenylpropane, 7.7 g of 98% acetic acid and 1.8 g of 98% sulphuric acid is stirred and refluxed at 130° to 138° C. while a mixture of 15.5 g of water, 4 ml of acetic acid and 0.5 ml of sulphuric acid is gradually added over the period of 2.5 h, after which time the hydrogen chloride evolution ceases. The work-up of the reaction mixture as described in Example 1 gives 33.6 g of cinnamic acid in 75.6% total yield (melting point 132° to 133° C., min. 99% purity). is gradually added over the period of 2.5 h

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

实验步骤: A mixture of 51.6 g of 1,1,1,3-tetrachloro-3-phenylpropane, 60 g of glacial acetic acid and 17.8 g of 55% sulphuric acid is refluxed under stirring at 115° to 122° C. for 5 h, after which time the evolution of hydrogen chloride ceases. The work-up of the reaction mixture as described in Example 1 yields 22.5 g and 2.9 g of cinnamic acid in 85.8% total yield (melting point 131.5° to 133° C., min. 99% purity). is refluxed

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

实验步骤: A mixture of 103.2 g of 1,1,1,3-tetrachloro-3-phenylpropane, 120 g of 85% formic acid and 17 g of Ostion KSC cation exchanger is refluxed at 100° to 105° C. for 7 h while hydrogen chloride and carbon monoxide is evolved. The cation exchanger is separated by filtration, the filtrate is cooled and the crystals precipitated are filtered off and washed with water to give 46.8 g of cinnamic acid in 79% chemical yield (melting point 127° to 133.5° C. and min. 97% purity). The cation exchanger is separated by filtration the filtrate is cooled the crystals precipitated are filtered off washed with water

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

实验步骤: A mixture of 103.2 g of 1,1,1,3-tetrachloro-3-phenylpropane, 114 g of 85% formic acid and 4.2 g of 93% sulphuric acid is refluxed under stirring at a temperature in the range 100° to 110° C. for 6 h with evolution of hydrogen chloride and carbon monoxide. The reaction mixture is cooled, the crystals so precipitated are filtered off and washed with water to give 51.5 g of cinnamic acid in total yield of 98 per cent (melting point 127° to 133° C., min. 98% purity). is refluxed The reaction mixture is cooled the crystals so precipitated are filtered off washed with water

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

实验步骤: A mixture of 129 g of 1,1,1,3-tetrachloro-3-phenylpropane and 100 g of 85% formic acid is heated to 100° to 106° C. for 10 h. Te reaction is accompanied by evolution of hydrogen chloride and carbon monoxide. Cooling the reaction mixture, filtration of the crystals and their washing with water affords 60 g of cinnamic acid in 81% yield (melting point 126° to 132° C., purity over 97per cent). is heated to 100° to 106° C. for 10 h Te reaction Cooling the reaction mixture, filtration of the crystals and their washing with water

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

实验步骤: A mixture of 129 g of 1,1,1,3-tetrachloro-3-phenylpropane, 74 g of glacial acetic acid and 39 g of Wolfatit OK 80 cation exchanger is heated to 118° to 124° C. for 15 h. The cation exchanger is removed from the hot reaction mixture by filtration. After cooling the mixture, filtration of the crystals and their washing with water, 56.5 g of cinnamic acid is obtained. Condensation of the filtrate followed by filtration of the crystals gives another 9.5 g of cinnamic acid with total yield of 89% (melting point after recrystallization 128° to 135° C., min. 98% purity). is heated to 118° to 124° C. for 15 h The cation exchanger is removed from the hot reaction mixture by filtration After cooling the mixture, filtration of the crystals and their washing with water

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

实验步骤: A mixture of 129 g of 1,1,1,3-tetrachloro-3-phenylpropane, 74 g of glacial acetic acid, and 31 g of monohydrate of p-toluenesulphonic acid is heated while stirring to the boiling point 115° to 120° C. for 13 h with gradual addition of 18 g of water. The precipitated crystals are filtered off, washed with water, to give 59 g of cinnamic acid. Then, the filtrate, is condensed, crystals are filtered off and washed with water to give another 11 g of cinnamic acid with the total yield of 94.5% (melting point 131° to 133° C., min. 98% purity). is heated The precipitated crystals are filtered off washed with water