Phosphorus pentachloride → HCID 19076174, compound

Participants

Reaction Conditions

Reaction Steps

Phosphorus pentachloride (40.55 g, 194.7 mmol) was added to a mixture of 7-carbomethoxy-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one 2 (14.23 g, 64.91 mmol) and xylene (200 mL) and was heated to 90° C. over a period of 15 min. After an additional 35 min at 90° C. the resulting solution was cooled to RT, filtered, concentrated, and saturated Na2CO3 (200 mL, aqueous) was added to the resulting oil. After stirring the mixture for 1.5 h the solid material was filtered and washed with EtOH (×2) then ether (×2) to give a mixture of 3. (LRMS (ES), [M+H] m/z=288) and a small amount of 1,3,3-trichloro-7-carbomethoxy-2,3,4,5-tetrahydro-1-benzazepin-2-one (13.60 g).

Provenance & Evidence