Water → HCID 20386489, Verbindung

HRID 46629

Reaktionsgleichung

Reaktionsgleichung von HRID 46629
C(O)(=[S:3])C.[OH-].[K+].Br[CH:8]1[CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[C:13]([Cl:17])[CH:14]=2)[C:9]1=[O:18].O>C(O)C>[Cl:17][C:13]1[CH:14]=[C:15]2[C:10](=[CH:11][CH:12]=1)[C:9](=[O:18])[CH:8]([SH:3])[CH2:16]2

Komponenten

6

Edukt 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 113340692-Bromo-5-chloro-2,3-dihydro-1H-inden-1-oneHCID 178418634HCID 178418634, Verbindung

Produkt 1

HCID 20386489HCID 20386489, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 1.37 g (18 mmoles) of thioacetic acid in 30 ml of ethanol is neutralized exactly, in a nitrogen atmosphere, by the dropwise addition of a 40% strength aqueous KOH solution, and 3.7 g (15 mmoles) of 2-bromo-5-chloro-1-indanone (Example 1 (a)) are added. The reaction mixture is stirred for 1 hour at room temperature and poured into 200 ml of water. The product which crystallizes after some time is filtered off and introduced, under nitrogen, into 35 ml of a 5% strength aqueous NaOH solution. After stirring for 1 hour at room temperature, the pH is adjusted to 1 with 2 N hydrochloric acid and the crystalline precipitate is filtered off. The resulting 5-chloro-2-mercapto-1-indanone decomposes at 173°-175° C.

Aufarbeitung

  1. additionare added
  2. customThe product which crystallizes after some time
  3. filtrationis filtered off
  4. additionintroduced, under nitrogen, into 35 ml of a 5% strength aqueous NaOH solution
  5. stirringAfter stirring for 1 hour at room temperature
  6. filtrationthe crystalline precipitate is filtered off
  7. customdecomposes at 173°-175° C.

Quellen und Nachweise

ORD-Eintrag
ord-4665f573712346a2b027cf886708c8c9
Quelldatensatz
uspto-grants-1979_11
Patentnummer
US04174397

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