反应详情

温度

60 °C

A stirred and cooled (0° C.) solution of 30 parts of 1-(4-amino-2-methoxyphenyl)ethanone in 360 parts of a concentrated hydrochloric acid solution, 75 parts of water and 30 parts of acetic acid is diazotated with a solution of 17.25 parts of sodium nitrite in 200 parts of water. After stirring for 30 minutes at 0° C., the whole is poured onto a solution of 30 parts of copper (I) chloride in 240 parts of a concentrated hydrochloric acid solution while stirring. The mixture is heated for 1 hour at 60° C. After cooling to room temperature, the product is extracted twice with 2,2'-oxybispropane. The combined extracts are washed successively with water, a diluted sodium hydroxide solution and again twice with water, dried, filtered and evaporated, yielding 28 parts (76%) of 1-(4-chloro-2-methoxyphenyl)ethanone; mp. 55° C.

1. stirringAfter stirring for 30 minutes at 0° C.
2. stirringwhile stirring
3. temperatureAfter cooling to room temperature
4. extractionthe product is extracted twice with 2,2'-oxybispropane
5. washThe combined extracts are washed successively with water
6. dry with materiala diluted sodium hydroxide solution and again twice with water, dried
7. filtrationfiltered
8. customevaporated