Reaktion #451508

Reaktionsgleichung

m-Aminobenzyl alcohol

2,2,2-trifluoroethylisothiocyanate

→

1-(3-hydroxymethylphenyl)-3-(2,2,2-trifluoroethyl)thiourea

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeVolatile material was evaporated in vacuo
2. 2
   Wascheneluted with ethyl acetate

Vorschrift

m-Aminobenzyl alcohol (0.123 g.) and 2,2,2-trifluoroethylisothiocyanate (0.141 g.) were heated under reflux in acetone (5 ml.) for 2 hours. Volatile material was evaporated in vacuo and the crude residue was fractionated on a silica gel column (20 cm.×1 cm. diameter) eluted with ethyl acetate to give 1-(3-hydroxymethylphenyl)-3-(2,2,2-trifluoroethyl)thiourea. The n.m.r. spectrum in CDCl3 using tetramethylsilane as internal standard (δ=0) had the following resonances (δ): 7.2 (4H, multiplet); 4.6 (2H, singlet); 4.3 (2H, multiplet).

Quelle