5-AMino-2-fluoro-benzeneacetic acid ethyl ester HCl synthesis

Yield:1239460-72-0 95%

Reaction Conditions:

with sulfuric acid at 80; for 1 h;Inert atmosphere;

Steps:

To a solution of 2-(5-amino-2-fluorophenyl)acetic acid (6.13 g, 36.2mmol) in ethanol (15mL) was added cone, sulfuric acid (2mL) dropwise. The reaction mixture was stirred under N₂ at 80 ⁰C for lhr. After the reaction mixture was cooled to RT and neutralized with aqueous Na₂Cθ3 to pH 7-8, the aqueous solution was extracted with ethyl acetate (3 x 10OmL). The combined organic layer was washed with brine, dried over Na₂SO₄ and evaporated under vacuum to afford ethyl 2-(5-amino-2-fluorophenyl)acetate as a yellow oil which was used for the next step without further purification (6.13 g, 95%).

References:

WO2010/91310,2010,A1 Location in patent:Page/Page column 99