Reaktion #50440

Reaktionsgleichung

3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide

potassium thiocyanate

18-crown-6

→

7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-thiocyano-phthalide

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe mixture is then filtered through Celite®
2. 2
   Einengenconcentrated by evaporation
3. 3
   Sonstigechromatographed with 30% ethyl acetate/n-hexane

Vorschrift

A mixture of 1.4 g of 3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see Example 85) and 0.46 g of potassium thiocyanate is heated in the presence of a spatula tip of 18-crown-6 in 15 ml of acetonitrile for 4 hours. The mixture is then filtered through Celite®, concentrated by evaporation and chromatographed with 30% ethyl acetate/n-hexane to yield 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-thiocyano-phthalide in the form of light-yellow crystals, m.p. 161°-163° C.

Quelle