2,4,6-Trifluoroaniline → N-Benzyl-2-(2,4,6-trifluoro-phenylamino)-acetamide

Temperatur

100 °C

A mixture of N-benzyl-2-chloroacetamide (700 mg—obtained as described for intermediate 1), DIPEA (0.76 mL) and 2,4,6-trifluoro-aniline (559 mg) in anhydrous DMF (5 mL) was stirred at 100° C. for 40 hours under a Nitrogen atmosphere. Then, more DIPEA (0.2 mL) was added and the mixture was heated to 100° C. for further 4 hours. After cooling to room temperature, the solution was diluted with AcOEt and washed with water and ice. The separated aqueous phase was extracted with further AcOEt (3×30 mL). The combined organic extracts were dried and concentrated in vacuo. The residue was purified by flash chromatography (CH/AcOEt from 8:2 to 6:4) to give the title compound (265 mg) as a beige solid.

1. temperaturethe mixture was heated to 100° C. for further 4 hours
2. temperatureAfter cooling to room temperature
3. washwashed with water and ice
4. extractionThe separated aqueous phase was extracted with further AcOEt (3×30 mL)
5. customThe combined organic extracts were dried
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography (CH/AcOEt from 8:2 to 6:4)

ORD-Eintrag

ord-626c79338a9e48f8986e663a161a5007

Quelldatensatz

uspto-grants-2007_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07214680B2