Reaktion #1147776

Reaktionsgleichung

(4-amino-3-iodophenyl)methanol

diethyl ethoxymethylenemalonate

→

diethyl 2-{[4-(hydroxymethyl)-2-iodoanilino]methylene}malonate

Lösungsmittel

CH2Cl2

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigechromatographed (Biotage flash 40M, eluant CH2Cl2
2. 2
   workup.ADDITIONProduct containing fractions
3. 3
   Sonstigecondensed

Vorschrift

A solution of (4-amino-3-iodophenyl)methanol (5.97 g) and diethyl ethoxymethylenemalonate (5.34 mL) is heated at 100° C. for 30 min. The reaction is cooled to room temperature. The resulting solid is dissolved in a mixture of CH2Cl2 and MeOH, adsorbed onto silica and chromatographed (Biotage flash 40M, eluant CH2Cl2, then 0.5% MeOH/CH2Cl2). Product containing fractions are combined and condensed to afford diethyl 2-{[4-(hydroxymethyl)-2-iodoanilino]methylene}malonate as a white solid, m.p. 152-154° C.

Quelle