Water → Maltol

HRID 25907

Reaktionsgleichung

Reaktionsgleichung von HRID 25907
O.[O:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH:7]([OH:9])[CH3:8].BrCl.C(O)C1[O:17]C=CC=1>O1CCCC1>[CH3:8][C:7]1[O:9][CH:6]=[CH:5][C:4](=[O:17])[C:3]=1[OH:2]

Komponenten

6

Edukt 4

HCID 962WaterHCID 7361Furfuryl AlcoholHCID 61697BROMINE CHLORIDE (BrCl)2×HCID 1072431-(2-Furyl)ethanol

Produkt 1

HCID 8369Maltol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-3976e93e59f741129ece8359aa74db65
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04147705

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