Hydrochloric Acid → HCID 22840185, compound

Participants

Reaction Steps

A solution of 300 mg of rel-α-{3(S)-[1(S)ethoxycarbonyl-5-(4-piperidyl)pentylamino]-2-oxo-6(R)-phenylperhydroazepin-1-yl}acetic acid dihydrochloride (prepared as described in Example 22) in 3.2 ml of a 1N aqueous solution of sodium hydroxide was stirred for 16 hours at room temperature, and then its pH value was adjusted to a value of 4.5 by adding 1N aqueous hydrochloric acid. The resulting precipitate was collected by filtration and dissolved again in water containing a small amount of acetic acid. The resulting solution together with the filtrate was poured onto a column pached with a porous resin HP-20 (Mitsubishi Kasei Kogyo Co., Ltd.) and eluted first with water and then with 20% v/v aqueous acetone. The fractions first eluted with water contained sodium chloride and acetic acid, whilst the fractions eluted next with 20% v/v aqueous acetone contained the title compound. The latter fractions were concentrated by evaporation under reduced pressure to give 223 mg of the title compound as a powdery substance.

Provenance & Evidence