Sodium Bicarbonate → HCID 70111769, compound

Participants

Reaction Steps

To a solution of (3aR*,10aS*)-9-benzyl-4-(benzamidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (0.18 g, 0.4 mmol) in acetic anhydride (20 mL) was added 10 mg of p-toluenesulfonic acid monohydrate. The mixture was refluxed for two hours. To the reaction mixture was added a saturated aqueous solution of sodium hydrogencarbonate, which was subjected to extraction with dichloromethane. The extract was washed with water, which was dried, followed by distilling off the solvent. The residue was purified silica-gel column chromatography (dichloromethane), followed by crystallization from diethylether to give 0.11 g (yield 58%) of the titled compound, m.p. 164-°166° C.

Provenance & Evidence