2-Propanethiol → 2-(Isopropylthio)benzaldehyde

Temperatur

50 °C

2-fluoro-benzaldehyde (2.00 g, 16.1 mmol), potassium carbonate (2.45 g, 17.1 mmol) and 2-propanethiol (1.35 g, 17.1 mmol) were dissolved in 10.0 mL, DMF in a 50 mL round-bottomed flask under dry nitrogen, topped with a reflux condenser. The reaction mixture was heated to 50° C. for 48 h. After cooling the mixture was added to 50 mL of saturated potassium carbonate solution, and the mixture was extracted with 3×50 mL portions of ether. The extracts were dried with magnesium sulfate and evaporated. The yellow oil residue of the crude product was further purified by chromatography on silica gel using 95:5 petroleum ether (60-80) and dichloromethane as eluent to afford a yellow oil (2.58 g, 89%).

1. customtopped with a reflux condenser
2. temperatureAfter cooling the mixture
3. extractionthe mixture was extracted with 3×50 mL portions of ether
4. dry with materialThe extracts were dried with magnesium sulfate
5. customevaporated
6. customThe yellow oil residue of the crude product was further purified by chromatography on silica gel using 95:5 petroleum ether (60-80) and dichloromethane as eluent

ORD-Eintrag

ord-d2e33ba4a20c43d39c2bd1c4e572ee96

Quelldatensatz

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08513151B2