Trifluoroacetic anhydride → 2-Bromo-4-fluorobenzonitrile

A solution of 10.9 g. (0.05 mole) of 2-bromo-4-fluorobenzamide in 50 ml. of dry pyridine is stirred and cooled in an ice-bath while 11.2 g. (0.0525 mole) of trifluoroacetic anhydride is added dropwise. After 2 hours at room temperature, the bulk of the solvent is evaporated under reduced pressure and the residue is dissolved in ether. Evaporation of the washed and dried ethereal extract under reduced pressure leaves the product as the residual solid. Sublimation at 55° C. and 0.05 mm. yields white crystals, m.p. 75°-76.5° C. A sample from a previous experiment was resublimed for analysis, m.p. 77°-78° C.

1. temperaturecooled in an ice-bath while 11.2 g
2. customthe bulk of the solvent is evaporated under reduced pressure
3. dissolutionthe residue is dissolved in ether
4. customEvaporation of the
5. washwashed
6. customdried ethereal
7. extractionextract under reduced pressure
8. customleaves the product as the residual solid
9. customat 55° C.
10. customyields white crystals, m.p. 75°-76.5° C

ORDレコード

ord-af1a3cbda2d341cd86e5068c19029d57

出典データセット

uspto-grants-1978_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04071570