Acetic Anhydride → HCID 67552039, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of ethyl 3-(2-fluoro-5-(4-morpholinylmethyl)phenyl)-3-oxopropanoate (Preparation 3, 20.0 g), triethylorthoformate (21.5 ML) and acetic anhydride (21.4 mL) is heated at 150° C. in a round-bottom flask equipped with a Dean-Stark trap and condenser. After 4 h, the remaining acetic acid and triethylorthoforrnate are distilled off by heating the mixture to 100° C. at 0.2 Torr for 1 hr, leaving 22.9 g of the title compound as an amber oil. The crude product is used as is in the subsequent transformations. Physical characteristics: 1H NMR (300 MHz, DMSO-d6) δ 7.85, 7.60-7.45, 7.23, 4.36-4.17, 4.09-3.99, 3.56, 3.49, 2.34, 1.29-1.11, 1.08-0.99; MS (ESI+) m/z 366 (M+H)+.

Provenance & Evidence