Hydrochloric Acid → (E)-N-[2-[(2-acetyl-4-pyridyl)amino]ethyl]-4,4,5,5,5-pentafluoro-pent-2-enamide

Temperatur

100 °C

(E)-4,4,5,5,5-Pentafluoro-N-[2-[[2-(2-methyl-1,3-dioxolan-2-yl)-4-pyridyl]amino]ethyl]pent-2-enamide (35 mg, 0.09 mmol) was dissolved in aceton (1 ml), 4M hydrochloric acid (0.5 ml) was added and the mixture was stirred in a closed vessel at 100° C. for 15 minutes with microwave heating. The mixture was diluted with water, extracted with ethyl acetate and the organic phase was washed with brine, dried over magnesium sulfate and evaporated to dryness. The resulting residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 2.5 mg (0.0071 mmol, 7.9%).

1. extractionextracted with ethyl acetate
2. washthe organic phase was washed with brine
3. dry with materialdried over magnesium sulfate
4. customevaporated to dryness
5. customThe resulting residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)
6. customto yield 2.5 mg (0.0071 mmol, 7.9%)

ORD-Eintrag

ord-e4c6eb12c2b64977ad65a8c908d34c59

Quelldatensatz

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08877934B2