反应详情

温度

0 °C

Then, 4.0 g of (+)-2-methylbutanoic acid chloride and 7 ml of nitrobenzene were charged into a flask and cooled to 0° C., to which was added 10.74 g (80 mmol) of aluminum chloride with stirring and further added a solution of 4.97 g (19.6 mmol) of (+) 2-methylbutanoic acid-4-biphenyl in 9 ml of nitrobenzene and then stirred at room temperature for 70 hours. Thereafter, the resulting mixture was added with 2 normal hydrochloric acid and ice and extracted with chloroform. The chloroform layer was washed with water, dried on anhydrous magnesium sulfate, and purified by a column chromatography of silica gel after the distillation off of the solvent to obtain 3.60 g (yield 54%) of oily 2-methylbutanoic acid-4-(2-methylbutanoyl) biphenyl. The NMR analytical values of this purified product were as follows.

1. stirringstirred at room temperature for 70 hours
2. extractionextracted with chloroform
3. washThe chloroform layer was washed with water
4. dry with materialdried on anhydrous magnesium sulfate
5. custompurified by a column chromatography of silica gel
6. distillationafter the distillation off of the solvent