تفاعل #2200628

معادلة التفاعل

trifluoroacetic anhydride

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

triethylamine

→

title compound

المردود 83.0%

2-Fluoro-5-trifluoromethoxy-benzonitrile

المردود 83.0%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled in an ice bath
2. 2
   أخرىwas kept <30° C
3. 3
   أخرىAfter 1 h at rt all volatiles were evaporated (40° C., 200 mbar)
4. 4
   أخرىThe oily residue was partitioned (ether/water)
5. 5
   تجفيفthe organic phase was dried (Na2SO4)
6. 6
   تركيزconcentrated
7. 7
   workup.DISTILLATIONDistillation (24 mbar, T=80-83° C.)

الإجراء التجريبي

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]+.

المصدر