Reaction #2186174

ord-d5060ff6341449469bde122d2eb6ba0a

Reaction equation

O=C(Cl)c1ccccc1
benzoyl chloride
CCC(CO)(CO)CO
trimethylolpropane
CCC(CO)(CO)CO.O=C(O)c1ccccc1.O=C(O)c1ccccc1.O=C(O)c1ccccc1
Trimethylolpropane Tribenzoate

Conditions

Temperature
100°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.STIRRINGthe resulting mixture was stirred for an additional 30 minutes
  2. 2
    OtherAfter completion of the reaction
  3. 3
    Otherwas lowered to room temperature
  4. 4
    Otherthe resulting precipitates
  5. 5
    Filtrationwere collected by filtration
  6. 6
    WashThereafter, washing
  7. 7
    workup.ADDITIONby adding ethyl acetate-pure water
  8. 8
    OtherSubsequently, the organic phase was collected
  9. 9
    workup.DISTILLATIONethyl acetate was distilled out under vacuum, whereby 126 parts by weight (at a yield of 85 percents) of white crystals
  10. 10
    Otherwere obtained

Procedure

While stirring, 71 parts by weight of benzoyl chloride were dripped over 30 minutes to a mixed solution of 45 parts by weight of trimethylolpropane and 101 parts by weight of triethylamine maintained at 100° C., and the resulting mixture was stirred for an additional 30 minutes. After completion of the reaction, the temperature was lowered to room temperature and the resulting precipitates were collected by filtration. Thereafter, washing was performed by adding ethyl acetate-pure water. Subsequently, the organic phase was collected and ethyl acetate was distilled out under vacuum, whereby 126 parts by weight (at a yield of 85 percents) of white crystals were obtained. The molecular weight of the resulting compound was 446.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07569259B2uspto-grants-2009_08