Ethyl 3-hydroxy-3-(4-methoxyphenyl)-2-methylpropanoate → Ethyl 3-(4-methoxyphenyl)-2-methylprop-2-enoate

HRID 461095Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 461095
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9](O)[CH:10]([CH3:16])[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:5][CH:4]=1.S([O-])(O)(=O)=O.[K+]>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]=[C:10]([CH3:16])[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:7][CH:8]=1

Komponenten

4

Edukt 2

HCID 312882Ethyl 3-hydroxy-3-(4-methoxyphenyl)-2-methylpropanoateHCID 516920Potassium bisulfate

Produkt 1

HCID 53711494Ethyl 3-(4-methoxyphenyl)-2-methylprop-2-enoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A mixture of 71.8 g (0.30 mole) of ethyl β-(p-methoxyphenyl)-β-hydroxy-α-methylpropionate is refluxed with 41.0 g (0.30 mole) of potassium hydrogen sulfate in 718 ml of benzene for 1 hour. The insoluble white crystals formed are filtered off, washed with benzene and the solvent of the filtrate is removed on evaporation. This is dissolved in 700 ml of ether. The ether solution is washed with 4 × 100 ml of cold water until neutral followed by 80 ml of saturated sodium chloride solution, then it is dried over magnesium sulfate for 1.5 hours and filtered. The solvent is removed on an evaporator to give ethyl p-methoxy-α-methylcinnamate.

Aufarbeitung

  1. customThe insoluble white crystals formed
  2. filtrationare filtered off
  3. washwashed with benzene
  4. customthe solvent of the filtrate is removed on evaporation
  5. dissolutionThis is dissolved in 700 ml of ether
  6. washThe ether solution is washed with 4 × 100 ml of cold water
  7. dry with materialit is dried over magnesium sulfate for 1.5 hours
  8. filtrationfiltered
  9. customThe solvent is removed on an evaporator

Quellen und Nachweise

ORD-Eintrag
ord-39daad5a7252463c95e3a8965db6eb2c
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04061771

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