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ChemicalBook CAS DataBase List 2-Bromo-5-fluorobenzenepropanoic acid

2-Bromo-5-fluorobenzenepropanoic acid synthesis

2synthesis methods
-

Yield:-

Reaction Conditions:

with hydrogen;5% rhodium-on-charcoal in methanol at 20; under 760.051 Torr; for 12 h;

Steps:

14
Reference Example 14 A solution of 2-bromo-5-fluorobenzaldehyde (1.5 g), malonic acid (1.5 g), and piperidine (0.07 ml) in pyridine (10 ml) was heated for 1 day under reflux. The reaction liquid was concentrated under reduced pressure, 1 N hydrochloric acid was then added thereto for neutralization, and crystallized precipitates were collected by filtration. This was dissolved in methanol (10 ml), and a 5% rhodium carbon catalyst (150 mg) was added thereto, followed by stirring at room temperature for 12 hours under a hydrogen atmosphere (1 atm). The insoluble materials was removed by filtration through Celite, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:1) to obtain a compound of Reference Example 14 (0.50 g) as a colorless solid.

References:

Astellas Pharma Inc. EP2042480, 2009, A1 Location in patent:Page/Page column 13