反应详情

温度

0 °C

A 0.5-liter three-neck flask equipped with a stirrer was purged with nitrogen gas, and 7.2 g (0.3mols) of sodium hydride and 250 ml of dewatered tetrahydrofuran were put thereinto in a nitrogen stream atmosphere. With stirring, the mixture was cooled to 0° C., and, while its temperature was kept cooled, 66 ml (0.3 mols) of di-n-butyl malonate was dropwise added thereto over a period of 30 minutes. After the addition, the mixture was heated up to room temperature, and 32 ml of cyclopentyl bromide was dropwise added thereto, and refluxed for 5 hours. After this was cooled to room temperature, 10 g of sodium hydride and 32 ml of cyclopentyl bromide were added thereto, and refluxed further for 8 hours. The resulting reaction mixture was washed with 200 ml of water, and subjected to distillation under reduced pressure to obtain 20 g of di-n-butyl cyclopentylmalonate. The yield was 23.5%.

1. customA 0.5-liter three-neck flask equipped with a stirrer
2. temperaturewhile its temperature was kept cooled
3. additionAfter the addition
4. temperaturethe mixture was heated up to room temperature
5. temperaturerefluxed for 5 hours
6. temperatureAfter this was cooled to room temperature
7. temperaturerefluxed further for 8 hours
8. customThe resulting reaction mixture
9. washwas washed with 200 ml of water
10. distillationsubjected to distillation under reduced pressure