反应详情

温度

-15 °C

A slurry of 2.30 (7.52 mmol) g 4-(4-phenoxyphenoxy)benzoic acid, 30 ml of thionyl chloride and 2 drops of N,N-dimethylformamide is refluxed under nitrogen atmosphere for 16 hours. Excess thionyl chloride is distilled to yield an oil, and 200 ml of anhydrous n-hexane is added. The solution is cooled to -15° C., and the resulting precipitate is filtered and dried under nitrogen atmosphere. The precipitate is dissolved in a minimum volume of hot n-hexane, the solution is filtered and the filtrate is cooled to -15° C. to yield 1.82 g (66 percent yield) of 4-(4-phenoxyphenoxy)benzoyl chloride having a melting point of 85° C. to 89° C. by DSC measurement.

1. temperatureis refluxed under nitrogen atmosphere for 16 hours
2. distillationExcess thionyl chloride is distilled
3. customto yield an oil, and 200 ml of anhydrous n-hexane
4. additionis added
5. filtrationthe resulting precipitate is filtered
6. customdried under nitrogen atmosphere
7. dissolutionThe precipitate is dissolved in a minimum volume of hot n-hexane
8. filtrationthe solution is filtered
9. temperaturethe filtrate is cooled to -15° C.