HCID 14502069, compound → HCID 14502070, compound

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Reaction Steps

315.34 g (1 mol) of 2-trifluoromethyl-7-(N-ethoxycarbonylmethylamino)-6,7,8,9-tetrahydro-[5H]-benzocycloheptene are heated at reflux for approximately 25 minutes in a mixture of 1000 ml of normal sodium hydroxide and 2200 ml of ethanol. The ethanol is then distilled off terminating under reduced pressure, and the aqueous phase is washed twice with 4000 ml of diethyl ether each time. The ethereal phases are washed with water again. 1000 ml of a normal hydrochloric acid solution are added to the combined aqueous phases. The precipitate obtained is collected and washed. 250 g of 2-trifluoromethyl-7-(N-carboxymethylamino)-6,7,8,9-tetrahydro-[5H]-benzocycloheptene are obtained, which sublimes above 260° C. (Yield 87%). By adding a stoichiometric amount of hydrochloric acid and recrystallising from water, the hydrochloride of this amino acid, which sublimes towards 220°-222° C., is obtained.

Provenance & Evidence