反应详情

温度

110 °C

A solution of 2-cyclobutylmethyl-malonic acid diethyl ester (4.68 g, 20.5 mmol) in ethanol (45.4 mL) was treated with a solution of potassium hydroxide (3.45 g, 61.5 mmol) in water (11.4 mL). The reaction was then heated to 110° C. overnight. After this time, the reaction was cooled to 25° C. and was concentrated in vacuo. The residue was diluted with water (50 mL) which was then acidified with a 2N aqueous hydrochloric acid solution and then extracted with a 90/10 methylene chloride/methanol solution (3×50 mL). The combined organics were dried over sodium sulfate, filtered and concentrated in vacuo to afford 2-cyclobutylmethyl-malonic acid (1.22 g, 34.7%) as a tan solid. This material was used without further purification.

1. temperatureAfter this time, the reaction was cooled to 25° C.
2. concentrationwas concentrated in vacuo
3. additionThe residue was diluted with water (50 mL) which
4. extractionextracted with a 90/10 methylene chloride/methanol solution (3×50 mL)
5. dry with materialThe combined organics were dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo