反应 #64744

ord-6733c848ab3a417fbc7b41988b3b42bc

反应条件

温度
-25°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to stand at room temperature
  2. 2
    其他When precipitation of product
  3. 3
    其他(1-2 hr)
  4. 4
    其他before collecting the solid product

实验过程

Aluminum trifluoroethoxide was prepared by treatment of a toluene solution of triethylaluminum (0.38M) with these equivalents of trifluoroethanol at -25° C. After gas evolution was complete, the reaction mixture was allowed to stand at room temperature. When precipitation of product appeared to be well-advanced (1-2 hr), the reaction mixture was cooled at -25° C. for 18 hr before collecting the solid product. From 1.76 mmol of Et3Al and 0.528 g trifluoroethanol was obtained 435 mg of white solid, mp 171°-172° C. 1H NMR (THF-d8): 4.1 (q, J=8). 19F NMR (THF-d8): -77.0 (bd s), trace signals at -76.3 and-77.7.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05414140uspto-grants-1995_05