Reaktion #526821

Reaktionsgleichung

trifluoroacetic acid ethyl ester

1,4,7-triazaheptane

→

1,7-Bis(trifluoroacetyl)-1,4,7-triazaheptane

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated by evaporation in a vacuum
2. 2
   SonstigeThe remaining oil is crystallized from hexane

Vorschrift

113.3 g (790 mmol) of trifluoroacetic acid ethyl ester is instilled in a solution of 41.14 g (390 mmol) of 1,4,7-triazaheptane in 350 ml of tetrahydrofuran at 0° C. and under nitrogen. It is allowed to stir overnight at room temperature, concentrated by evaporation in a vacuum. The remaining oil is crystallized from hexane. Yield: 115 g (99.9% of theory) Melting point: 68°-70° C. Elementary analysis: Cld: C 32.55 H 3.76 F 38.62 N 14.24 Fnd: C 32.63 H 3.75 F 38.38 N 14.19

Quelle