反应详情

温度

130 °C

70 g (0.37 mmol) of diethyl methylmalonate dissolved in 50 cm3 of H2O-free EtOH were added dropwise at room temperature to 8.5 g (0.37 mmol) of sodium in 100 cm3 of H2O-free EtOH. 110 g (0.37 mmol) of 26 in 200 cm3 of H2O-free EtOH were subsequently added dropwise, and the mixture was refluxed for 3 hours. 62 g (1.1 mol) of KOB dissolved in 100 cm3 of H2O were added at room temperature, and the mixture was refluxed for a further 4 hours. The solvent was removed in vacuo, H2O was added to the residue until the latter had dissolved completely, and the mixture was acidified to pH 1 by means of concentrated aqueous HCl. The precipitate which had formed was filtered off with suction, dried and heated at 130° C. for 1 hour, giving 90 g (84%) of 27 as a viscous oil.

1. temperaturethe mixture was refluxed for 3 hours
2. additionwere added at room temperature
3. temperaturethe mixture was refluxed for a further 4 hours
4. customThe solvent was removed in vacuo, H2O
5. additionwas added to the residue until the latter
6. dissolutionhad dissolved completely
7. customThe precipitate which had formed
8. filtrationwas filtered off with suction
9. customdried