Potassium Hydroxide → HCID 86760732, Verbindung

Temperatur

120 °C

KOH (0.223 g, 3.97 mmol) was added to a solution of (2R)-1,1,1-trifluoro-2-(2-mercapto-1,3-thiazol-5-yl)butan-2-ol (0.966 g, 3.97 mmol) in dry MeOH. When a solution was obtained, the reaction mixture was concentrated to dryness. Dry toluene was then added and the mixture was concentrated to dryness again. The residue was dissolved with 7-bromo-4-pyridin-3-yl-2H-chromen-2-one (1.0 g, 3.31 mmol) in NMP, and the resulting mixture was stirred at 120° C. for 16 h. Once cooled, the mixture was directly applied onto a column of silica gel and chromatographed (acetone/toluene; 5:95 to 15:85), affording the title compound. 1H NMR (400 MHz, CDCl3): δ 8.81 (dd,1H), 8.72 (dd, 1H), 7.82 (dt, 1H), 7.78 (s, 1H), 7.51-7.59 (m, 2H), 7.33-7.40 (m, 2H), 6.42 (s, 1H), 2.88 (br s, 1H), 2.12 (q, 2H), 0.99 (t, 3H).

1. customWhen a solution was obtained
2. concentrationthe reaction mixture was concentrated to dryness
3. additionDry toluene was then added
4. concentrationthe mixture was concentrated to dryness again
5. temperatureOnce cooled
6. customchromatographed (acetone/toluene; 5:95 to 15:85)

ORD-Eintrag

ord-2e40798ca1194e008a5d0ed2827612fa

Quelldatensatz

uspto-grants-2008_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07439260B2