반응 #74840

반응 방정식

p-fluorobenzoylacetonitrile

trimethyl orthoacetate

acetic anhydride

→

title compound

2-(p-Fluorobenzoyl)-3-methoxycrotononitrile

반응 조건

후처리

1. 1
   workup.ADDITIONA solution containing 55.8 g
2. 2
   온도to reflux for 5 hours
3. 3
   기타The excess solvent and volatile by-products are then removed by vacuum distillation
4. 4
   기타the residue is recrystallized from diethyl ether
5. 5
   workup.DISTILLATIONAlternatively, the distillation residue may be distilled over on a Kugelrohr apparatus at 160° C./0.25 mm
6. 6
   기타to provide a viscous oil which
7. 7
   기타may be crystallized from diethyl ether

실험 절차

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.

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