Reaktion #50455

Reaktionsgleichung

7-hydroxy-3-methyl-phthalide

Lawesson reagent

→

7-hydroxy-3-methylisobenzofuran-1(3H)-thione

Lösungsmittel

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationChromatographic filtration of the mixture on silica gel (eluant

Vorschrift

3.9 g of 7-hydroxy-3-methyl-phthalide (see Examples 101 and 111) and 5.1 g of Lawesson reagent are heated in 20 ml of xylene for 4 hours at 140° C. Chromatographic filtration of the mixture on silica gel (eluant: ethyl acetate/n-hexane (1:9)] yields 7-hydroxy-3-methylisobenzofuran-1(3H)-thione, m.p. 39°-41° C.; IR spectrum (CHCl3): C=O 1624, 1604, 1368, 1330, 1304, 1165 cm-1 ; mass spectrum: 180 (M+ =100), 165(58), 137(24).

Quelle