반응 #54185

반응 방정식

furfuryl alcohol

BrCl

BrCl

1(2-furyl)-1-ethanol

water

→

maltol

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONis added via a gas inlet tube
2. 2
   workup.ADDITIONThe rate of addition
3. 3
   온도while maintaining the temperature below 30° C
4. 4
   온도The reaction mixture is heated
5. 5
   온도to reflux
6. 6
   기타the tetrahydrofuran removed by distillation
7. 7
   기타reaches 105° C.
8. 8
   온도the reaction mixture heated
9. 9
   온도under reflux for about 2 hours
10. 10
    온도The reaction mixture is cooled

실험 절차

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.

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