HCID 11794316, Verbindung → HCID 9840907, Verbindung

HRID 849897Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 849897
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[C:9]([S:22][C:23]2[CH:33]=[CH:32][C:26]([C:27](OCC)=[O:28])=[CH:25][CH:24]=2)=[CH:10][C:11]2[C:12]([CH3:21])([CH3:20])[CH2:13][CH2:14][C:15]([CH3:19])([CH3:18])[C:16]=2[CH:17]=1>C1COCC1>[CH3:7][C:8]1[C:9]([S:22][C:23]2[CH:33]=[CH:32][C:26]([CH2:27][OH:28])=[CH:25][CH:24]=2)=[CH:10][C:11]2[C:12]([CH3:21])([CH3:20])[CH2:13][CH2:14][C:15]([CH3:18])([CH3:19])[C:16]=2[CH:17]=1

Komponenten

4

Edukt 2

HCID 11794316HCID 11794316, VerbindungHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 9840907HCID 9840907, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

144 mg (3.8 mmol) of lithium aluminum hydride and 50 ml of THF were introduced into a three-necked flask and under a nitrogen stream. Next, a solution of 1.4 g (3.8 mmol) of ethyl 4-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthylthio)benzoate in 25 ml of THF was introduced dropwise and the mixture was heated at reflux for 8 hours. The excess hydride was destroyed with a potassium sodium tartrate solution and the reaction medium was extracted with ethyl acetate. The organic phase was decanted off, dried over magnesium sulfate and evaporated.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 8 hours
  3. customThe excess hydride was destroyed with a potassium sodium tartrate solution
  4. extractionthe reaction medium was extracted with ethyl acetate
  5. customThe organic phase was decanted off
  6. dry with materialdried over magnesium sulfate
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f710d02a37844321a938e8a7c3f33027
Quelldatensatz
uspto-grants-2000_01
Patentnummer
US06015569

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