Ethanol → HCID 18983531, compound

HRID 1440367Notes

Reaction equation

HRID 1440367 reaction equation
[C:1]1([P:7]([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:14][O:15][C:16]1[CH:21]=CC(O)=[CH:18][CH:17]=1.C(O)C>>[C:1]1([P:7]([O:11][C:12]2[CH:18]=[CH:17][C:16]([O:15][CH3:14])=[CH:21][CH:13]=2)[O:8][CH2:9][CH3:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 3

HCID 702EthanolHCID 90154-MethoxyphenolHCID 74225Diethyl phenylphosphonite

Product 1

HCID 18983531HCID 18983531, compound

Conditions

Temperature
160 °C

Procedure

99 g (0.5 mol) of diethyl phenylphosphonite and 62 g (0.5 mol) of 4-methoxyphenol were mixed and heated with stirring at 415 mbar. Ethanol distilled off at 115° C. via a small column. The temperature was then increased stepwise to 160° C., and the vacuum was simultaneously increased to 70 mbar. In total, 21.5 g (0.467 mol) of ethanol distilled off. The batch was then cooled and distilled. After a first fraction of 29 g, which essentially contained the unreacted starting materials, 103 g were obtained having a boiling point from 135° to 138° C. at 0.1 to 0.2 mbar. The yield was thus 75% of theory.

Workup

  1. temperatureheated
  2. distillationEthanol distilled off at 115° C. via a small column
  3. temperaturethe vacuum was simultaneously increased to 70 mbar
  4. temperatureThe batch was then cooled
  5. distillationdistilled
  6. custom103 g were obtained
  7. customfrom 135° to 138° C.

Sources & evidence

ORD record
ord-897c88b5931d4faa9d17af11e45b3cbc
Source dataset
uspto-grants-1996_03
Patent number
US05498741

Reaction notes

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