反应详情

温度

70 °C

To toluene (100 ml), sodium hydroxide (16.7 g, 418 mmol) and 2-dimethylamino-2-methyl-1-propanol (23.4 g, 200 mmol) were added and the mixture was heated at reflux for 2 hours. After cooling to 70° C., β-dimethylaminoethyl chloride hydrochloride (28.8 g, 200 mmol) was added. Then, the mixture was heated at reflux for 5.5 hours. After cooling to room temperature, insolubles were separated by filtration and the organic phase was concentrated under reduced pressure. The residue was distilled under reduced pressure to obtain 10.3 g (in a yield of 27%) of the objective compound as a colorless liquid.

1. temperaturethe mixture was heated
2. temperatureat reflux for 2 hours
3. temperatureThen, the mixture was heated
4. temperatureat reflux for 5.5 hours
5. temperatureAfter cooling to room temperature
6. custominsolubles were separated by filtration
7. concentrationthe organic phase was concentrated under reduced pressure
8. distillationThe residue was distilled under reduced pressure