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0 °C

A suspension of 5.24 g of AlCl3 and 0.52 g of ZnCl2 in 40 ml of 1,2-dichloroethane is cooled to 0° C., and a solution of 5.0 g of 2,4-dimethoxytoluene in 20 ml of 1,2-dichloroethane is added dropwise. The mixture is then cooled to -10° C., and a solution of 2.9 ml of chloroacetyl chloride in 1.5 ml of 1,2-dichloroethane is added dropwise while the temperature of the reaction medium is maintained at between -10° C. and -7° C. The mixture is left stirring while the temperature is allowed to rise to r.t., the reaction medium is poured into a mixture of ice and concentrated HCl, the resulting mixture is extracted with DCM, the combined organic phases are washed with water and dried over magnesium sulphate and the solvents are evaporated off under vacuum. The residue is taken up in heptane and the precipitate formed is filtered off. 3.0 g of the expected product, m.p.=166°-167° C., are obtained.

1. temperatureThe mixture is then cooled to -10° C.
2. temperatureis maintained at between -10° C. and -7° C
3. waitThe mixture is left
4. customto rise to r.t.
5. extractionthe resulting mixture is extracted with DCM
6. washthe combined organic phases are washed with water
7. dry with materialdried over magnesium sulphate
8. customthe solvents are evaporated off under vacuum
9. customthe precipitate formed
10. filtrationis filtered off