Hydrochloric Acid → HCID 66840740, Verbindung

Temperatur

65 °C

To 4-chlorobenzaldehyde 46a (99.6 mmol, 14 g) in water (44 mL) was added KOH (44.6 mmol, 2.5 g). The mixture was heated at 65° C. and 3-pentanone (99.6 mmol, 8.58 g) was added dropwise over 10 min. After refluxing for 8 h, the reaction mixture was cooled to room temperature and stirred overnight. Following addition of 260 mL 1N aqueous HCl, the mixture was extracted with EtOAc. The organic layer was dried over Na2SO4 and concentrated. The crude product was purified by flash column chromatography (silica gel, 5% EtOAc/heptane) to give 8.59 g of 46b.

1. temperatureAfter refluxing for 8 h
2. temperaturethe reaction mixture was cooled to room temperature
3. extractionthe mixture was extracted with EtOAc
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated
6. customThe crude product was purified by flash column chromatography (silica gel, 5% EtOAc/heptane)

ORD-Eintrag

ord-2e03c952bbf0490e87b8c293cd22cedc

Quelldatensatz

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08722658B2