Yield:39629-86-2 97%

Reaction Conditions:

in water at 110; for 30 h;Sealed tube;

Steps:

49

INTERMEDIATE 49 - PREPARATION OF δ-oxo-i-phenylpyrrolidine-S-carboxylic acid.; A mixture of aniline (3.26 g; 34.68 mmol) and 2-methylenesuccinic acid (5.47 g; 41.62 mmol) in water (10 ml) was heated in a sealed tube at 1 10 ⁰C for 30 hours. After cooling to room temperature, 6N NaOH (13 mL) was added and the resulting precipitate was filtered off. The filtrate was acidified with 6N hydrochloric acid to pH 1 and the resulting precipitate was filtered, washed with water, and dried to yield 6.92 g (97%) of 5-oxo-1- phenypyrrolidine-3-carboxylic acid as a white solid. ESI/APCI(+): 206 (M+H), 228 (M+Na).ESI/APCK-): 204 (M- H).

References:

WO2010/142801,2010,A1 Location in patent:Page/Page column 161