Reaktion #2136850

Reaktionsgleichung

potassium

thiobenzoic acid

chloromethyl thiocyanate

→

thiobenzoic acid chloromethyl ester

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated
2. 2
   Extraktionthe residue was extracted
3. 3
   workup.STIRRINGby shaking with water/ethylene chloride
4. 4
   Einengenthe organic phase was concentrated
5. 5
   Temperaturby heating to 80°-100°/0.5 to 2 mm Hg for several hours

Vorschrift

28 g (0.16 mol) of the potassium salt of thiobenzoic acid were dissolved in 550 ml of methanol, and 17 g (0.16 mol) of chloromethyl thiocyanate were added dropwise at -5°. After slowly warming the reaction mixture to room temperature, it was subsequently stirred at 40° for a further 30 minutes and concentrated, the residue was extracted by shaking with water/ethylene chloride, the organic phase was concentrated and the oily residue was freed from chloromethyl thiocyanate residues by heating to 80°-100°/0.5 to 2 mm Hg for several hours; yield 30 g (this corresponds to a yield of 90% of the theretical conversion).

Quelle