Dichloromethane → 2-Bromo-4-ethoxycarbonyl(methanesulfonyloxy) methyl-1,7-di(trimethylsilylethoxymethyl)-6,7-dihydropyrrolo [2,3-c]azepin-8-one

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Reaction Steps

A 0.046 ml amount of methanesulfonyl chloride was dropwise added under ice cooling to a 5 ml methylene chloride solution of 295 mg of the compound (13) synthesized in Example 3 and 0.21 ml of triethylamine. The mixture was stirred at room temperature for 1 hour. A saturated aqueous solution of sodium hydrogen carbonate was added thereto and extraction was performed with methylene chloride. The extract was washed with saturated saline, dried, filtered, and concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (hexane:ether=2:3) to obtain 331 mg of the above-referenced compound (15) (yield 99%).

Provenance & Evidence