Reaction #1435691

ord-ff41d439271049cc87c22c19283a3591

Reaction equation

CCOC(=O)C(F)(F)F
trifluoroacetic acid ethyl ester
NCCNCCN
1,4,7-triazaheptane
O=C(NCCNCCNC(=O)C(F)(F)F)C(F)(F)F
1,7-Bis(trifluoroacetyl)-1,4,7-triazaheptane

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Concentrationconcentrated by evaporation in a vacuum
  2. 2
    OtherThe remaining oil is crystallized from hexane

Procedure

113.3 g (790 mmol) of trifluoroacetic acid ethyl ester is added in drops to a solution consisting of 41.14 g (390 mmol) of 1,4,7-triazaheptane in 350 ml of tetrahydrofuran at 80° 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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07211241B2uspto-grants-2007_05