Diethyl phosphate → Diethyl 2-hydroxyethyl phosphate

HRID 620445

反応式

HRID 620445 の反応式
[P:1]([OH:9])([O:6][CH2:7][CH3:8])([O:3][CH2:4][CH3:5])=[O:2].[CH2:10]1[O:12][CH2:11]1>>[P:1]([O:9][CH2:10][CH2:11][OH:12])([O:6][CH2:7][CH3:8])([O:3][CH2:4][CH3:5])=[O:2]

参加物

3

反応物 2

HCID 654Diethyl phosphateHCID 6354Ethylene Oxide2 回

生成物 1

HCID 14892894Diethyl 2-hydroxyethyl phosphate

実験手順

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

後処理

  1. customA 2 liter, 3-necked flask was equipped with a Dewar condenser, gas inlet
  2. additionwere added over a 4 hour period
  3. custom(pot temperature 50° C.) acid number=70
  4. additiontemperature dropped to 40° C.
  5. distillationdistilled at 80° C.

出典と根拠

ORDレコード
ord-bee792810ad5435488aeb1b5054a7835
出典データセット
uspto-grants-1989_04
特許番号
US04820854

関連ノート

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