反应 #2186174

ord-d5060ff6341449469bde122d2eb6ba0a

反应方程式

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

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe resulting mixture was stirred for an additional 30 minutes
  2. 2
    其他After completion of the reaction
  3. 3
    其他was lowered to room temperature
  4. 4
    其他the resulting precipitates
  5. 5
    过滤were collected by filtration
  6. 6
    洗涤Thereafter, washing
  7. 7
    workup.ADDITIONby adding ethyl acetate-pure water
  8. 8
    其他Subsequently, 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
    其他were obtained

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07569259B2uspto-grants-2009_08