2-bromo-4-fluorobenzamide

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. cooled in an ice-bath while 11.2 g the bulk of the solvent is evaporated under reduced pressure the residue is dissolved in ether Evaporation of the washed dried ethereal extract under reduced pressure leaves the product as the residual solid at 55° C. yields white crystals, m.p. 75°-76.5° C

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 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. cooled in an ice-bath while 11.2 g the bulk of the solvent is evaporated under reduced pressure the residue is dissolved in ether Evaporation of the washed dried ethereal extract under reduced pressure leaves the product as the residual solid at 55°C. yields white crystals, m.p. 75°-76.5°C