Acetic Acid → HCID 68417859, compound

Participants

Reaction Steps

To a solution of methyl-5-cyano-2-(2-methoxy-2-oxoethoxy)benzoate (5 g, 0.02 mol) in methanol (1 L) was added glacial acetic acid (1.1 g, 0.02 mol) and passed N2 for 30 min. To this was added Pd/C (1.5 g, 35%) and hydrogenated under 2.5 Kg of pressure for 24 h. The reaction mixture was filtered and filtrate concentrated under vacuum (temp. 38° C. under N2). To the crude residue was added 100 mL of EtOAc and again removed under vacuum at same temp. The solid was treated with 100 mL EtOAc, stirred for 2 h, filtered and dried to give the title compound as a white powder (2.25 g, 35%). TLC: chloroform/methanol, 9:1, Rf: 0.15

Provenance & Evidence