反应 #2200628

反应方程式

trifluoroacetic anhydride

E-2-fluoro-5-trifluoromethoxy-benzaldehyde oxime

triethylamine

→

title compound

收率 83.0%

2-Fluoro-5-trifluoromethoxy-benzonitrile

收率 83.0%

溶剂

THF

反应条件

后处理

1. 1
   温度The mixture was cooled in an ice bath
2. 2
   其他was kept <30° C
3. 3
   其他After 1 h at rt all volatiles were evaporated (40° C., 200 mbar)
4. 4
   其他The oily residue was partitioned (ether/water)
5. 5
   干燥the organic phase was dried (Na2SO4)
6. 6
   浓缩concentrated
7. 7
   workup.DISTILLATIONDistillation (24 mbar, T=80-83° C.)

实验过程

To a solution of E-2-fluoro-5-trifluoromethoxy-benzaldehyde oxime (47.5 g, 213 mmol) in THF (400 ml) was added triethylamine (65.0 ml, 466 mmol). The mixture was cooled in an ice bath and trifluoroacetic anhydride (32.8 ml, 236 mmol) was added at such a rate that the temperature was kept <30° C. After 1 h at rt all volatiles were evaporated (40° C., 200 mbar). The oily residue was partitioned (ether/water), the organic phase was dried (Na2SO4) and concentrated. Distillation (24 mbar, T=80-83° C.) afforded the title compound (36.1 g, 83%) that was sufficiently pure to be used in the next step. MS: m/e=205 [M]+.

来源