2-Mercaptobenzoic Acid → Sodium Thiosalicylate

HRID 1287524Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1287524
[SH:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[H-].[Na+:12]>COCCOC>[SH:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O-:6])=[O:5].[Na+:12]

Komponenten

4

Edukt 2

HCID 54432-Mercaptobenzoic AcidHCID 24758Sodium hydride

Produkt 1

HCID 23690429Sodium ThiosalicylateAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80711,2-DimethoxyethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A solution of 2-mercaptobenzoic acid (15.4 g, 0.1 mole) in 50 ml of 1,2-dimethoxyethane (DME) was slowly added, with cooling, to a stirred suspension of 0.1 mole of sodium hydride in DME, the suspension having been prepared by washing 4.2 grams of a 57% oil dispersion with dry n-hexane (3 times) and replacing the last wash with dry 1,2-dimethoxyethane (50 ml). Cooling was necessary to maintain the temperature below 25°C. The resultant suspension was heated at 50°C for 2 hours, cooled to 0°C and filtered. The solid was washed well with cold DME (ca. 50 ml) and dried under vacuum overnight to yield sodium 2-mercaptobenzoate: 17.6 g (100% yield);

Aufarbeitung

  1. customthe suspension having been prepared
  2. washby washing 4.2 grams of a 57% oil dispersion with dry n-hexane (3 times)
  3. washlast wash with dry 1,2-dimethoxyethane (50 ml)
  4. temperatureCooling
  5. temperatureto maintain the temperature below 25°C
  6. temperaturecooled to 0°C
  7. filtrationfiltered
  8. washThe solid was washed well with cold DME (ca. 50 ml)
  9. customdried under vacuum overnight

Quellen und Nachweise

ORD-Eintrag
ord-c303460bb8464f50bb0787f26390e585
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03984573

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