Bromoacetyl bromide → HCID 70111628, compound

Participants

Reaction Steps

To a solution of bromoacetyl bromide (0.29 mL, 3.3 mmol) in dichloromethane (5 mL) was added dropwise a solution of (3aR*,10aS*)-9-(2-phenylethyl)-2,3,3a,4,9,10a- hexahydrobenzo [b]cyclopenta[e][1,4]diazepin-10(1H)-one (0.92 g, 3.0 mmol) in dichloromethane (5 mL). The solution was stirred for 3 hours at room temperature. To the reaction mixture was added a saturated aqueous solution of sodium hydrogencarbonate. The aqueous layer was separated, and the organic layer was washed with water and a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and subjected to filtration. The filtrate was concentrated under reduced pressure. The concentrate was purified by silica-gel column chromatography (hexane - ethyl acetate 5:1,then 1:1) to afford the desired product (924 mg, 72%). Oily product.

Provenance & Evidence