Hydrochloric Acid → 3-Hydroxy-2-methoxy-1,2-diphenylpropan-1-one

HRID 851851

Reaktionsgleichung

Reaktionsgleichung von HRID 851851
[OH-:1].[K+].[CH3:3][O:4][CH:5]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[CH2:20]=O.Cl>C(O)C.O.CS(C)=O>[CH3:3][O:4][C:5]([CH2:20][OH:1])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 14797Potassium HydroxideHCID 98097Methyl Benzoin

Produkt 1

HCID 219095133-Hydroxy-2-methoxy-1,2-diphenylpropan-1-one

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 679Dimethyl SulfoxideLösungsmittelHCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Potassium hydroxide 0.4 g was dissolved in ethanol 5 mL and dimethyl sulfoxide 200 mL was further added to obtain a solution. Benzoin methyl ether 30 g (0.13 mol) was dissolved in the solution and paraformaldehyde 5 g (0.16 mol) was added and reacted at 40° C. for 3 hours under nitrogen current. After that, the reaction product was cooled to a room temperature and neutralized with a dilute hydrochloric acid and then saturated salt water 120 mL was added. The solution was extracted by ethyl acetate and the extracted liquid was washed with saturated salt water three times. The washed product was dried and concentrated by anhydrous magnesium sulfate and recrystallized by diethyl ether. α-methylol benzoin methyl ether (MBME) was obtained in such a manner.

Aufarbeitung

  1. customto obtain a solution
  2. additionwas added
  3. customreacted at 40° C. for 3 hours under nitrogen current
  4. extractionThe solution was extracted by ethyl acetate
  5. washthe extracted liquid was washed with saturated salt water three times
  6. customThe washed product was dried
  7. concentrationconcentrated by anhydrous magnesium sulfate
  8. customrecrystallized by diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-7a309612a73f478487bc80aaed6533eb
Quelldatensatz
uspto-grants-2007_08
Patentnummer
US07253131B2

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