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温度

0 °C

6.80 g (38 mmol) of 2-methyl-2-phenyl-propionic acid methyl ester was dissolved at rt in 200 mL MeCl2 and 7.01 ml (90.4 g=76 mmol) of dichloromethylmethylether was added and the mixture cooled down to 0° C.; 21.47 mL (36.93 g=191 mmol) TiCl4 was added over 15 min and the reaction warmed up to ambient temperature; stirring was continued for 16 hours. The reaction mixture was then treated at 0° C. with 20 ml of HCl (37% in water) and extracted twice with MeCl2; the organic phases were washed with water, dried over MgSO4, filtered and evaporated. The crude product was purified by chromatography (silicagel, eluent:gradient of n-heptane/EtOAc) to yield 5.00 g of the title compound as yellow oil. MS: 206.1 (M+).

1. temperaturethe reaction warmed up to ambient temperature
2. extractionextracted twice with MeCl2
3. washthe organic phases were washed with water
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated
7. customThe crude product was purified by chromatography (silicagel, eluent:gradient of n-heptane/EtOAc)