1,1,2,2-tetrachloroethene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:75.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: α,α,α'-Trichloro-m-xylene (22.5 grams, 93.2% a.i., 0.1 moles) was dissolved in 18 mls. of tetrachloroethylene. Hexachloroethane (59.2 grams, 0.25 moles), potassium hydroxide (12.8 grams, 87.7%, 0.2 moles), water (2.13 grams), and dodecyltrimethylammonium chloride (0.255 grams, 0.001 moles) were added. The mixture was heated at 75° C. for 2.5 hours with good stirring. The reaction was quenched with 30 mls. of water and 18 mls tetrachloroethylene. The organic phase was separated and washed with water. The excess solvent and hexachloroethane were distilled off to give an 85.2% yield of α,α,α,α'-tetrachloroxylene with a purity of 84%. , 0.1 moles) was dissolved in 18 mls The reaction was quenched with 30 mls The organic phase was separated washed with water The excess solvent and hexachloroethane were distilled off

反応条件: temp:75.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: α,α,α'-Trichloro-m-xylene (22.5 grams, 93.2% a.i., 0.1 moles) was dissolved in 18 mls. of tetrachloroethylene. Hexachloroethane (59.2 grams, 0.25 moles), potassium hydroxide (12.8 grams, 87.7%, 0.2 moles), water (2.13 grams), and dodecyltrimethylammonium chloride (0.255 grams, 0.001 moles) were added. The mixture was heated at 75° C. for 2.5 hours with good stirring. The reaction was quenched with 30 mls. of water and 18 mls tetrachloroethylene. The organic phase was separated and washed with water. The excess solvent and hexachloroethane were distilled off to give an 85.2% yield of α,α,α,α'-tetrachloroxylene with a purity of 84%. , 0.1 moles) was dissolved in 18 mls The reaction was quenched with 30 mls The organic phase was separated washed with water The excess solvent and hexachloroethane were distilled off

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of ethyl 1-(7-chloroquinazolin-4-yl)-5-hydroxy-2-methylindol-3-ylacetate (1.0g.) in dry dimethyl-formamide (10ml.); dried by distillation from calcium hydride, and stored over sodium alumino-silicate) was added to sodium hydride (0.068g.), and the mixture was stirred under a slight vacuum (ca 150mm. Hg) at room temperature for 15 minutes. n-Propyl iodide (0.9g.) was added to the resulting clear solution, and the mixture stirred at room temperature overnight. The solution was added to water (300ml.) and extracted with ethyl acetate (3 × 40ml.). The combined extracts were washed with a saturated solution of sodium chloride (30ml.), dried (MgSO4), and then evaporated in vacuo. The yellow oil thus obtained was treated with tetrachloroethylene (100ml.) and the solution evaporated in vacuo. This process was then replaced with ethanol (50ml.) to give ethyl 1-(7chloroquinazolin-4-yl)-2-methyl-5-n-propoxyindol-3-ylacetate as a stiff yellow syrup [NMR: 2-CH3 at 7.65 τ; pure by TLC (systems A and D)]. dried by distillation from calcium hydride was added to sodium hydride (0.068g.) n-Propyl iodide (0.9g.) was added to the resulting clear solution the mixture stirred at room temperature overnight The solution was added to water (300ml.) extracted with ethyl acetate (3 × 40ml.) The combined extracts were washed with a saturated solution of sodium chloride (30ml.) dried (MgSO4) evaporated in vacuo The yellow oil thus obtained the solution evaporated in vacuo

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Appropriate operating conditions of a dividing wall column will depend on the separation desirably being conducted therein, and those of ordinary skill in the art of chemical engineering are readily able to determine the same. For the exemplary reaction of methyl chloride and perchloroethylene to provide 1,1,2,3-tetrachloropropene, wherein methyl chloride, methylene chloride, chloroform, perchloroethylene, and 1,1,2,3-tetrachloropropene are desirably separated, suitable operating conditions for the dividing wall column include a pressure of about 266 psia and temperature of about 91° C. at the feed stream, a pressure of about 63 psia and a temperature of about 16° C. at the overhead, and a pressure of about 68 psia and a temperature of about 186° C. at the column bottom. will depend on the separation For the exemplary reaction of methyl chloride and perchloroethylene

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Another aspect of this invention is a method of preheating chemical reaction vessels prior to start of operations of an exothermic reaction so that the reactor can be heated from ambient conditions to the temperature at which the exothermic reaction can be initiated and maintained during operation. Preferably, there is provided a chemical reaction vessel having at least two heating assemblies as described hereinabove which are switched to the on position for reactor preheat of about 2000 amps and 10-15 volts and left until the temperature reaches that desired. Then the heating assemblies are switched off and the reactor feed is allowed to enter the feed inlet and upon contacting the hot environment of the reactor the desired reaction occurs and the products and byproducts, if any, are allowed to leave via the crude product outlet. Typical examples of such processes are carried out in thermal chlorinators which produce methyl chloride, methylene chloride, trichloromethane, perchloroethylene, trichloroethylene, allyl chloride and the like. chemical reaction vessels to start of operations of an exothermic reaction so that the reactor can be heated from ambient conditions to the temperature at which the exothermic reaction maintained during operation Preferably, there is provided a chemical reaction vessel left until the temperature reaction

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Another aspect of this invention is a method of preheating chemical reaction vessels prior to start of operations of an exothermic reaction so that the reactor can be heated from ambient conditions to the temperature at which the exothermic reaction can be initiated and maintained during operation. Preferably, there is provided a chemical reaction vessel having at least two heating assemblies as described hereinabove which are switched to the on position for reactor preheat of about 2000 amps and 10-15 volts and left until the temperature reaches that desired. Then the heating assemblies are switched off and the reactor feed is allowed to enter the feed inlet and upon contacting the hot environment of the reactor the desired reaction occurs and the products and byproducts, if any, are allowed to leave via the crude product outlet. Typical examples of such processes are carried out in thermal chlorinators which produce methyl chloride, methylene chloride, trichloromethane, perchloroethylene, trichloroethylene, allyl chloride and the like. chemical reaction vessels to start of operations of an exothermic reaction so that the reactor can be heated from ambient conditions to the temperature at which the exothermic reaction maintained during operation Preferably, there is provided a chemical reaction vessel left until the temperature reaction