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温度

0 °C

To a stirred and refluxing Grignard-complex, previously prepared starting from 7.3 parts of magnesium, 52.6 parts of methyl iodide in 160 parts of ether, is added dropwise a solution of 19.6 parts of 3'-bromo-2'-methylbenzonitrile in 40 parts of ether. Upon completion, stirring at reflux is continued for 20 hours. The reaction mixture is cooled to 0° C and poured onto 500 parts of ice-water while stirring vigorously. The ethereal phase is separated, dried and evaporated. The residue is boiled in 60 parts of a 6N hydrochloric acid solution for 10 minutes. The separated oil is extracted with ether. The extract is washed with water, dried and evaporated. The residue is distilled, yielding 3'-bromo-2'- methylacetophenone; bp. 125°-128°C at 10 mm. pressure.

1. temperaturerefluxing Grignard-complex
2. custompreviously prepared
3. stirringUpon completion, stirring
4. temperatureat reflux
5. stirringwhile stirring vigorously
6. customThe ethereal phase is separated
7. customdried
8. customevaporated
9. waitThe residue is boiled in 60 parts of a 6N hydrochloric acid solution for 10 minutes
10. extractionThe separated oil is extracted with ether
11. washThe extract is washed with water
12. customdried
13. customevaporated
14. distillationThe residue is distilled