Reaction #2075692

ord-57dac3167d2a4aaebbb490b8439bd5d0

Reaction equation

NCCCNCCCN
3,3′-iminobispropylamine
CCOC(=O)C(F)(F)F
ethyl trifluoroacetate
O=C(NCCCNCCCNC(=O)C(F)(F)F)C(F)(F)F
2,2,2-trifluoro-N-{3-[3-(2,2,2-trifluoroacetylamino)propylamino]propyl}acetamide

Conditions

Temperature
0°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONAt the end of the addition (3 hours later), the reaction mixture
  2. 2
    Otherto return to room temperature
  3. 3
    Temperaturethe stirring was maintained for a few hours under argon

Procedure

35 g of 3,3′-iminobispropylamine (266.7 mmol) were solubilized in 150 ml of anhydrous tetrahydrofuran under an argon stream. The reaction mixture was then cooled to 0° C. on an ice bath and 65 ml of ethyl trifluoroacetate (546.8 mmol) were added dropwise (very slowly) using a dropping funnel. At the end of the addition (3 hours later), the reaction mixture was allowed to return to room temperature and the stirring was maintained for a few hours under argon.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07641914B2uspto-grants-2010_01