反应详情

温度

5 °C

To a solution of 72.9 g (0.455 mol) of isobutylmalonic acid in 650 ml of ethyl acetate 54.2 ml (38.3 g, 0.524 mol) of diethylamine was added dropwise at 5° C. To the obtained suspension 19.2 g (0.640 mol) of paraform was added. The resulting mixture was refluxed for 5 h, then cooled to 5° C., and 350 ml of ether and 1000 cm3 of 2M HCl were added. After mixing the organic layer was separated, the aqueous layer was additionally extracted with 2×500 ml of ether. The combined organic extract was dried over Na2SO4 and then evaporated to dryness. Rectification of the residue in vacuum gave the title product, bp 75-77° C./6 mm Hg. Yield 51.5 g (88%) of colorless liquid.

1. temperatureThe resulting mixture was refluxed for 5 h
2. additionAfter mixing the organic layer
3. customwas separated
4. extractionthe aqueous layer was additionally extracted with 2×500 ml of ether
5. extractionThe combined organic extract
6. dry with materialwas dried over Na2SO4
7. customevaporated to dryness