Sulfuric Acid → 90103-48-3

HRID 542908

Reaktionsgleichung

Reaktionsgleichung von HRID 542908
[CH3:1][C:2]1([CH3:27])[C:10]2[CH:9]=[C:8]([C:11]([CH3:24])=[CH:12][C:13]3[CH:23]=[CH:22][C:16]([C:17]([O:19]CC)=[O:18])=[CH:15][CH:14]=3)[S:7][C:6]=2[C:5]([CH3:26])([CH3:25])[CH2:4][CH2:3]1.[OH-].[K+].S(=O)(=O)(O)O>C(O)C.O>[CH3:1][C:2]1([CH3:27])[C:10]2[CH:9]=[C:8](/[C:11](/[CH3:24])=[CH:12]/[C:13]3[CH:14]=[CH:15][C:16]([C:17]([OH:19])=[O:18])=[CH:22][CH:23]=3)[S:7][C:6]=2[C:5]([CH3:26])([CH3:25])[CH2:4][CH2:3]1

Komponenten

6

Edukt 3

HCID 1118Sulfuric AcidHCID 14797Potassium HydroxideHCID 53678243Ethyl p-[2-(4,5,6,7-tetrahydro-4,4,7,7-tetramethylbenzo[b]thien-2-yl)propenyl]-benzoate

Produkt 1

HCID 643976390103-48-3Ausbeute 86,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

3.0 g of ethyl p-[2-(4,5,6,7-tetrahydro-4,4,7,7-tetramethylbenzo[b]thien-2-yl)propenyl]benzoate are dissolved in 100 ml of ethanol and the solution is treated with a solution of 3.9 g of potassium hydroxide in 20 ml of water. After stirring at 50° C. for 3 hours, the mixture is cooled, poured into ice-water and acidified with 2N sulphuric acid. The mixture is extracted with ethyl acetate, the organic phase is washed with water, dried over sodium sulphate and evaporated. After recrystalization of the residue from ethyl acetate, there are obtained 2.4 g of p-[(E)-2-(4,5,6,7-tetrahydro-4,4,7,7-tetramethylbenzo[b]thien-2-yl)propenyl]benzoic acid in the form of pale yellowish crystals, m.p. 236°-238° C.

Aufarbeitung

  1. temperaturethe mixture is cooled
  2. extractionThe mixture is extracted with ethyl acetate
  3. washthe organic phase is washed with water
  4. dry with materialdried over sodium sulphate
  5. customevaporated
  6. customAfter recrystalization of the residue from ethyl acetate, there

Quellen und Nachweise

ORD-Eintrag
ord-e3936f81073c4ac3b9f4e5c38b14f997
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04659735

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