Phenolphthalein → HCID 53988615, Verbindung

HRID 247183

Reaktionsgleichung

Reaktionsgleichung von HRID 247183
[C:1]([OH:4])(=[S:3])[CH3:2].C1C=CC2C(C3C=CC(O)=CC=3)(C3C=CC(O)=CC=3)OC(=O)C=2C=1.C([O-])([O-])=O.[K+].[K+].[CH2:35]([O:37][C:38](=[S:48])[CH2:39][CH2:40][CH2:41][CH2:42][CH:43](Br)[CH2:44][CH2:45][CH3:46])[CH3:36]>O>[CH2:35]([O:37][C:38](=[S:48])[CH2:39][CH2:40][CH2:41][CH2:42][CH:43]([S:3][C:1](=[O:4])[CH3:2])[CH2:44][CH2:45][CH3:46])[CH3:36]

Komponenten

6

Edukt 4

HCID 4764PhenolphthaleinHCID 11430Potassium CarbonateHCID 544334916-Bromo-8-methylthiooctanoic acid ethyl esterHCID 178418634HCID 178418634, Verbindung

Produkt 1

HCID 53988615HCID 53988615, VerbindungAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

8.6 grams (0.113 mole) of thioacetic acid in 20 ml of water-free ethanol were neutralized to phenolphthalein with 81 ml of 10% ethanolic potash solution (0.113 mole potassium hydroxide) and 29.7 grams (0.1 mole) of 6-bromo-8-methylthiooctanoic acid ethyl ester added. The mixture was heated at reflux for 6 hours in a nitrogen atmosphere and allowed to stand for 10 hours at room temperature. The precipitated potassium bromide was filtered off, the filtrate concentrated in a vacuum, the residue taken up in 300 ml of diethyl ether and filtered, the filtrate was washed twice, each time with 100 ml of water, dried with sodium sulfate and concentrated in a vacuum. There were obtained 26 grams (89% of theory) of crude 6-acetylthio-8-methylthiooctanoic acid ethyl ester.

Aufarbeitung

  1. additionadded
  2. temperatureThe mixture was heated
  3. temperatureat reflux for 6 hours in a nitrogen atmosphere
  4. filtrationThe precipitated potassium bromide was filtered off
  5. concentrationthe filtrate concentrated in a vacuum
  6. filtrationfiltered
  7. washthe filtrate was washed twice
  8. dry with materialeach time with 100 ml of water, dried with sodium sulfate
  9. concentrationconcentrated in a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-3bb1d4b26ea2489f8d8eeb05e663aaff
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04705867

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