diethyl hydrogen phosphate

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR26## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR26## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 H2O acid number=4.8 to methyl red HCl/H2O acid number=12.6 to methyl red Thus, the compound has the structure ##STR27## A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR26## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 H2O acid number=4.8 to methyl red HCl/H2O acid number=12.6 to methyl red Thus, the compound has the structure ##STR27## A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR28## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 H2O acid number=4.8 to methyl red HCl/H2O acid number=12.6 to methyl red Thus, the compound had the structure ##STR29## A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR28## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 H2O acid number=4.8 to methyl red HCl/H2O acid number=12.6 to methyl red Thus, the compound had the structure ##STR29## A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 100 parts by weight of diethyl hydrogen phosphite and 50 parts by weight of phosphoric acid are mixed and reacted. The reaction is exothermic and the temperature of the reactants are keep below their boiling point for 30 minutes to 1 hour thereby producing a diethyl hydrogen-phosphoric acid compound. reacted for 30 minutes to 1 hour

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR26## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR26## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet and stirring bar. 875 grams (5.7 mole) of diethyl hydrogen phosphate was placed into the flask and about 400 grams of ethylene oxide were added over a 4 hour period. When the exotherm slowed, (pot temperature 50° C.) acid number=70. After the exotherm ceased and temperature dropped to 40° C., acid number=about 50. After refluxing of the ethylene oxide at 50° C. for 1 hour, acid number=about 18, after 3 hours at 50° C. acid number=about 7. All the above acid numbers were based on methyl red end point titration. The total yield was 1171 grams. Approximately half of the product was then wipe film distilled at 80° C. and 0.5 millimeter Hg. NMR data showed a compound having the formula: ##STR26## acid number=1.7 to methyl red, 6.7 to PNB HCl acid to methyl red=14.3 to phenolphthalein=16.3 H2O acid number=4.8 to methyl red HCl/H2O acid number=12.6 to methyl red Thus, the compound has the structure ##STR27## A 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet were added over a 4 hour period (pot temperature 50° C.) acid number=70 temperature dropped to 40° C. distilled at 80° C.