反应详情

温度

0 °C

To a 3-neck round bottom flask is charged a solution of 50 ml of water and 20 ml of tetrahydrofuran and the solution is cooled to 0° C. An addition funnel is charged with a solution of 1(2-furyl)-1-ethanol (0.89 mole) in 25 ml of tetrahydrofuran and this solution is added dropwise to the reaction flask while BrCl (0.30 mole) is added via a gas inlet tube. The rate of addition is such that all the furfuryl alcohol is added in the first 1.3-1.5 equivalents of BrCl while maintaining the temperature below 30° C. The reaction mixture is heated to reflux and the tetrahydrofuran removed by distillation. When the temperature reaches 105° C., a condensor is attached and the reaction mixture heated under reflux for about 2 hours. The reaction mixture is cooled and maltol isolated by the method of Example 1.

1. additionis added via a gas inlet tube
2. additionThe rate of addition
3. temperaturewhile maintaining the temperature below 30° C
4. temperatureThe reaction mixture is heated
5. temperatureto reflux
6. customthe tetrahydrofuran removed by distillation
7. customreaches 105° C.
8. temperaturethe reaction mixture heated
9. temperatureunder reflux for about 2 hours
10. temperatureThe reaction mixture is cooled