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Water → HCID 178454905, compound

HRID 488074
Notes
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Reaction equation

HRID 488074 reaction equation
[CH2:1]([P:5]([CH2:21][CH2:22][CH2:23][CH3:24])[O:6]C1C=CC(C(C)(C)C)=CC=1C(C)(C)C)[CH2:2][CH2:3][CH3:4].O>C(#N)C>[CH2:1]([PH:5](=[O:6])[CH2:21][CH2:22][CH2:23][CH3:24])[CH2:2][CH2:3][CH3:4]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 962WaterHCID 190917302.4-Di-tert.-butylphenyl dibutylphosphinite

Product 1

HCID 178454905HCID 178454905, compoundYield 70%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Conditions

Temperature
70 °C

Procedure

35 g (0.1 mol) of 2.4-di-tert.-butylphenyl dibutylphosphinite from Example 5 were reacted in 100 ml of acetonitrile with 2.0 g (0.11 mol) of water at 20° C., and the mixture was then stirred at 70° C. for 1 hour. The solvent was distilled off in vacuo, 50 ml of water and 100 ml of ethyl acetate were added, the phases were separated, and the organic phase was extracted two more times with 50 ml each of water. The combined aqueous phases were evaporated, and the residue distilled in vacuo, giving 10.2 g (70%) of a colorless liquid having a boiling point of 102° to 104° C./0.25 mbar.

Workup

  1. distillationThe solvent was distilled off in vacuo, 50 ml of water and 100 ml of ethyl acetate
  2. additionwere added
  3. customthe phases were separated
  4. extractionthe organic phase was extracted two more times with 50 ml each of water
  5. customThe combined aqueous phases were evaporated
  6. distillationthe residue distilled in vacuo

Sources & evidence

ORD record
ord-de33f1bfd5ca4255822885dfb4d95eb7
Source dataset
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05298644

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes