反应详情

温度

-40 °C

An amount of 26 mL (198 mmol) of Lithium diiopropylamide (Aldrich) is added to a three neck flask cooled to −40° C. To this is added drops wise, a mixture of 4-tert-butyl-2-methyl-benzoic acid 1.9 g (9.9 mmol) and dimethyl carbonate 3.3 mL (39.6 mmol) in 5 mL of tetrahydrofuran, while keeping the temperature at −60° C. After the addition, the temperature is kept between −40° C. to −60° C. for four hours, then brought to 0° C. and quenched with 25 mL of water. The mixture is allowed to stir at room temperature for two hours and acidify to pH 2 with hydrogen chloride, extracted 3× with ethyl acetate, dried over magnesium sulfate and evaporated.

1. additionTo this is added drops wise
2. customat −60° C
3. additionAfter the addition
4. custombrought to 0° C.
5. customquenched with 25 mL of water
6. extractionextracted 3× with ethyl acetate
7. dry with materialdried over magnesium sulfate
8. customevaporated