反应详情

A mixture of 30 parts of methyl benzeneacetate, 6.8 parts of sodium hydride dispersion 78%, 135 parts of N,N-dimethylformamide and 180 parts of benzene is stirred for 1 hour at room temperature, while nitrogen gas is introduced. Another 90 parts of benzene is added. Then there is added dropwise, during a 30 minutes-period, a solution of 43.4 parts of 1,3-dichloro-4-(chloromethyl)benzene in 45 parts of N,N-dimethylformamide. Upon completion, stirring is continued for 30 minutes at room temperature. The reaction mixture is poured onto water and the product is extracted twice with 2,2'-oxybispropane. The combined extracts are washed with water, dried, filtered and evaporated. The residue is distilled, yielding 26.5 parts of methyl 2,4-dichloro-α-phenylbenzenepropanoate; bp. 140°-145° C at 0.05 mm. pressure.

1. additionis introduced
2. additionThen there is added dropwise, during a 30 minutes-period
3. stirringUpon completion, stirring
4. waitis continued for 30 minutes at room temperature
5. additionThe reaction mixture is poured onto water
6. extractionthe product is extracted twice with 2,2'-oxybispropane
7. washThe combined extracts are washed with water
8. customdried
9. filtrationfiltered
10. customevaporated
11. distillationThe residue is distilled