反应详情

A solution containing 55.8 g. (0.34 mole) of p-fluorobenzoylacetonitrile, 41 g. (0.34 mole) of trimethyl orthoacetate, and 90 g. (0.88 mole) of acetic anhydride is heated to reflux for 5 hours. The excess solvent and volatile by-products are then removed by vacuum distillation and the residue is recrystallized from diethyl ether. Alternatively, the distillation residue may be distilled over on a Kugelrohr apparatus at 160° C./0.25 mm. to provide a viscous oil which may be crystallized from diethyl ether to provide the pure title compound.

1. additionA solution containing 55.8 g
2. temperatureto reflux for 5 hours
3. customThe excess solvent and volatile by-products are then removed by vacuum distillation
4. customthe residue is recrystallized from diethyl ether
5. distillationAlternatively, the distillation residue may be distilled over on a Kugelrohr apparatus at 160° C./0.25 mm
6. customto provide a viscous oil which
7. custommay be crystallized from diethyl ether