Diphenyl Ether → 3-(8-Chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)-4-[(4-pyridinylmethyl)amino]-3-cyclobutene-1,2-dione, hydrochloride

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Reaction Steps

A mixture of the product of Example 5 (0.75 g), 4-(aminomethyl)pyridine (0.14 mL) and diphenylether (2 mL) was heated to reflux for 3 hours. The mixture was cooled and added to hexane (200 mL) and the separated thick oil was recovered by decantation. The oil was triturated with methanol. The precipitated solid was filtered and stirred with methanol at ambient temperature for 16 hours. The solid was then filtered and dissolved in CHCl3 (4 mL). To the solution was added 7 N HCl (1 mL) and the mixture was concentrated in vacuo. The residue was triturated with ether and filtered to obtain the title compound as a yellow solid.

Provenance & Evidence