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Hydrochloric Acid → ST51001684

HRID 325258
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 325258
[Na].C(OCC)(=O)[CH2:3][C:4](OCC)=[O:5].[CH2:13]([S:15][CH:16]([CH3:23])[CH2:17][CH:18]=[CH:19][C:20](=[O:22])[CH3:21])[CH3:14].[OH-].[Na+].Cl>O.C(O)C>[CH2:13]([S:15][CH:16]([CH3:23])[CH2:17][CH:18]1[CH2:3][C:4](=[O:5])[CH2:21][C:20](=[O:22])[CH2:19]1)[CH3:14]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 7761Diethyl MalonateHCID 14798Sodium Hydroxide2×HCID 5360545SodiumHCID 544576116-Ethylthio-3-hepten-2-one

Produkt 1

HCID 3116068ST51001684

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

2.53 g of metallic sodium were added to 100 ml of ethanol at room temperature. To this was then added 17.6 g of diethyl malonate, with stirring, and then 17.2 g of 6-ethylthio-3-hepten-2-one was added. The resulting mixture was then refluxed for four hours and then an aqueous sodium hydroxide solution, containing 9.5 g of sodium hydroxide in 75 ml of water, was added and the mixture refluxed for another two hours. The mixture was cooled to 50° C. and then acidified by the addition of concentrated hydrochloric acid. The mixture was then warm until decarboxylation was complete and then evaporated to a liquid residue. The residue was mixed with ethyl ether, washed with water, and evaporated to a brown liquid. The liquid was base, acid extracted affording 5-(2-ethylthiopropyl) cyclohexane-1,3-dione.

Aufarbeitung

  1. temperatureThe resulting mixture was then refluxed for four hours
  2. additionwas added
  3. temperaturethe mixture refluxed for another two hours
  4. temperatureThe mixture was then warm until decarboxylation
  5. customevaporated to a liquid residue
  6. additionThe residue was mixed with ethyl ether
  7. washwashed with water
  8. customevaporated to a brown liquid
  9. extractionextracted

Quellen und Nachweise

ORD-Eintrag
ord-df045bf557ba463696722405c7f3092f
Quelldatensatz
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04440566

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