Triacetoxyperiodinane → HCID 18185015, Verbindung

The above 5-trifluoromethyl-indan-2-yl-methanol (216 mg, 1 mmol) was dissolved in methylene chloride (15 mL) and the solution was cooled in an ice bath. To this solution was added Dess-Martin reagent (450 mg, 1.06 mmol) in four portions. The mixture was warmed to room temperature and stirred for 1 hr. The mixture was evaporated to dryness and the residue was triturated with petroleum ether (14 mL) and ether (7 mL). The precipitate was filtered out and the filtrate was extracted with ether and sodium bicarbonate solution. The organic layer was dried over sodium sulfate and solvents were evaporated to give 5-trifluoromethyl-indan-2-carbaldehyde (210 mg) as pale green oil. 1H-NMR (CDCl3) □ 9.78 (s, 1H), 7.48 (s, 1H), 7.43 (d, 1H), 7.32 (d, 1H), 3.33-3.38 (m, 3H), 3.15-3.27 (m, 2H).

1. temperaturethe solution was cooled in an ice bath
2. customThe mixture was evaporated to dryness
3. customthe residue was triturated with petroleum ether (14 mL) and ether (7 mL)
4. filtrationThe precipitate was filtered out
5. extractionthe filtrate was extracted with ether and sodium bicarbonate solution
6. dry with materialThe organic layer was dried over sodium sulfate and solvents
7. customwere evaporated

ORD-Eintrag

ord-c025d9911ba5488c975d39755884a3b3

Quelldatensatz

uspto-grants-2010_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07652053B2