Sodium Acetate → HCID 19076181, compound

Participants

Reaction Steps

A 10% Pd/C mixture (0.9 g) was added to a mixture of 3,3-dichloro-7-carbomethoxy-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one 3 and 1,3,3-trichloro-7-carbomethoxy-2,3,4,5-tetrahydro-1-benzazepin-2-one (9.34 g), NaOAc (5.51 g, 40.5 mmol), and glacial acetic acid (25 mL). After stirring under a hydrogen atmosphere (balloon) at RT for 3.5 h and at 60° C. for an additional 30 min, the reaction mixture was filtered (celite) and concentrated. The resulting material was partitioned between saturated NaHSO4 (aqueous) and CH2Cl2. The organic layer was removed and the aqueous layer was extracted with CH2Cl2 (×2). The combined organic extracts were dried (Na2SO4) and concentrated to give 4 (3.6 g). LRMS (ES), [M+H] m/z=254.

Provenance & Evidence