2-丙基-1,3-二氧戊环

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter stirred autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155°C. by passing steam through internal coils. After about 3 1/2 minutes the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18°C. yields about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 3 1/2 minutes the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18°C.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155°C. by passing steam through internal coils. After about 31/2 minutes the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18°C. yields about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 31/2 minutes the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18°C.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155°C. by passing steam through internal coils. After about 31/2 minutes the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18°C. yields about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 31/2 minutes the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18°C.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter stirred autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155° C. by passing steam through internal coils. After about 31/2 minutes the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18° C. yields about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 31/2 minutes the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18° C.

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

实验步骤: The mixture consisting of 50 g (0.431 moles) of 2-propyl-1,3-dioxolane and 250 g of ethylene glycol is hydrogenolyzed in a mechanically agitated autoclave of 1-liter capacity, in the presence of 9 mg of hydroquinone, 5 g of palladium catalyst deposited on carbon at a rate of 5% of palladium by weight and of 210 mg of concentrated phosphoric acid. After 3 hours at a temperature of 170° C. under a hydrogen pressure kept constant at 30 bars, the degree of conversion of the 2-propyl dioxolane reaches 98.2%; 46.1 g (0.390 moles) of 2-butoxy-1-ethanol are produced besides 2.35 g (0.0135 moles) of 1,2-dibutoxy ethane and 0.31 g (0.004 moles) of normal butanol.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 2-liter stirred autoclave was charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) was then pumped in and the reactor heated quickly to 155°C. by passing steam through internal coils. After about 31/2 minutes the reaction was terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide was flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18°C. gave about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 31/2 minutes the reaction was terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18°C.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter stirred autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155°C. by passing steam through internal coils. After about 31/2 minutes, the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18°C. gives about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 31/2 minutes, the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18°C.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter stirred autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155°C. by passing steam through internal coils. After about 3 1/2 minutes the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18°C. yields about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 3 1/2 minutes the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18°C.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155°C. by passing steam through internal coils. After about 31/2 minutes the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18°C. yields about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 31/2 minutes the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18°C.

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 3-liter stirred autoclave is charged with 600 grams of crude terephthalic acid (3.61 moles), 1600 ml. of 2-propyldioxolane reaction medium, 0.11 mole of tetraethyl ammonium terephthalate catalyst and then purged with nitrogen. Liquid ethylene oxide (473 grams, 10.75 mole) is then pumped in and the reactor heated quickly to 155° C. by passing steam through internal coils. After about 31/2 minutes the reaction is terminated by pressuring the contents of the autoclave into a vessel where the ethylene oxide is flashed and then the unreacted terephthalic acid removed by filtration. Cooling of the filtrate to about 18° C. yields about 742 grams of crude bis(2-hydroxyethyl) terephthalate. purged with nitrogen After about 31/2 minutes the reaction is terminated the unreacted terephthalic acid removed by filtration Cooling of the filtrate to about 18° C.