반응 #2186174

ord-d5060ff6341449469bde122d2eb6ba0a

반응 방정식

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

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe resulting mixture was stirred for an additional 30 minutes
  2. 2
    기타After completion of the reaction
  3. 3
    기타was lowered to room temperature
  4. 4
    기타the resulting precipitates
  5. 5
    여과were collected by filtration
  6. 6
    세척Thereafter, washing
  7. 7
    workup.ADDITIONby adding ethyl acetate-pure water
  8. 8
    기타Subsequently, 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
    기타were obtained

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07569259B2uspto-grants-2009_08