Water → HCID 10160441, Verbindung

5-Chloro-1-(5-methanesulfonyl-pyridin-2-yl)-3-trifluoromethyl-1H-pyrazole-4-carbonitrile (0.35 g, 1 mmol) and (4-methylene-cyclohexyl)-methanol (0.252 g, 2 mmol) were dissolved in dry dimethylsulfoxide (DMSO) (5 ml) and potassium fluoride (0.116 g, 2 mmol) was added to the clear solution. The resulting mixture was stirred at 20° for a period of 48 hours. Analytical HPLC indicated the reaction completion. The reaction mixture was poured into water (50 ml) and the resulting mixture was extracted with ethyl acetate (20 ml). The organic extract was dried over magnesium sulfate and concentrated with a rotary evaporator. The desired product (0.3 g, 68%) was isolated by chromatography on silica gel eluting with a solution of 15% of ethyl acetate and 15% of acetone in hexane. MS: 440, r.t.: 3.0.

1. extractionthe resulting mixture was extracted with ethyl acetate (20 ml)
2. extractionThe organic extract
3. dry with materialwas dried over magnesium sulfate
4. concentrationconcentrated with a rotary evaporator

ORD-Eintrag

ord-8d9ab7bd44374d7886b8846bcb39788b

Quelldatensatz

uspto-grants-2004_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06794512B2