Sodium Hydroxide → 2-(4-Chloro-2-methylphenyl)benzoic acid

Temperature

100 °C

A mixture of ethyl 4′-chloro-2′-methyl-biphenyl-2-carboxylate (27.10 g), ethanol (60 ml) and 1N aqueous sodium hydroxide solution (120 ml) was stirred at 100° C. for 2 hr. To the reaction mixture was added 8N aqueous sodium hydroxide m solution (10 ml), and the mixture was further stirred at 100° C. for 1 hr. The reaction mixture was cooled to room temperature. The insoluble material was filtered off, and washed with 33 v/v % ethanol-water (100 ml). The filtrate was adjusted to pH 2 with formic acid (23 ml) and the mixture was stirred at room temperature for 1 hr. This suspension was filtered, and the obtained solid was air-dried for 1 hr and dried under reduced pressure at 60° C. to give the title compound (22.082 g, 91%).

1. stirringthe mixture was further stirred at 100° C. for 1 hr
2. temperatureThe reaction mixture was cooled to room temperature
3. filtrationThe insoluble material was filtered off
4. washwashed with 33 v/v % ethanol-water (100 ml)
5. stirringthe mixture was stirred at room temperature for 1 hr
6. filtrationThis suspension was filtered
7. customthe obtained solid was air-dried for 1 hr
8. customdried under reduced pressure at 60° C.

ORD record

ord-33c55c85fa584a568ef58d3c9a9c3cb5

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08871934B2