HCID 14976589, compound → HCID 14976590, compound

Polyphosphoric acid (35 g) was heated to melt at 120 C for 30 minutes. To this was added 1.2 g (5.1 mmol) 4-(2,3-dichlorophenyl)butanoic acid (PC68) and this mixture was heated further with stirring for 10 h at 130 C. LCMS analysis showed the formation of the product and the disappearance of starting material. The reaction mixture was then cooled and water (100 ml) was added. It was then extracted with ethylacetate (100 ml) and then was washed with Saturated Sodium bicarbonate (50 ml). The organic phase was dried and evaporated in vacuum. The oily residue was subjected to column chromatography with Hexane-ethylacetate (98:2) to obtain the tetralone as a yellow solid.

1. temperaturethis mixture was heated further
2. temperatureThe reaction mixture was then cooled
3. extractionIt was then extracted with ethylacetate (100 ml)
4. washwas washed with Saturated Sodium bicarbonate (50 ml)
5. customThe organic phase was dried
6. customevaporated in vacuum

ORD record

ord-af9ee6e9a92c4f5fa007a320a9a6ee92

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08969573B2