HCID 59726037, compound → HCID 59726039, compound

Participants

Reaction Conditions

Reaction Steps

Iron powder (18.2 g, 330 mmol) was added to a solution of methyl ester 2-2 (13.3 g, 480 mmol) in glacial acetic acid (120 mL). The mixture was stirred at 55° C. for 1.5 h and then filtered hot through celite, washing with ethyl acetate. The filtrate was concentrated then ethyl acetate and sat. aq. NaCO3 were added. The organic layer was isolated, washed with H2O, dried over K2CO3 and concentrated to give 2-3 as an off-white solid (11.6 g, 97% yield). 1H NMR (CDCl3, 400 MHz) δ 3.79 (s, 3H), 3.89 (s, 3H), 6.71 (s, 1H).

Provenance & Evidence