Hydrochloric Acid → HCID 178456462, compound

Participants

Reaction Conditions

Reaction Steps

The same procedure as in Example 2 was repeated using 1.96 g (3.44 mmol) of the mixture of Compound l and Compound m to give a crude product. The crude product was dissolved in 50 ml of methanol, and 1.5 ml of 1N hydrochloric acid was added to the solution, followed by stirring at 50° C. for 2 hours. After the solution was concentrated to about a half of its original volume, the concentrate was adjusted to pH 4 and extracted six times with chloroform. The organic layers were combined and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: 10% methanol/chloroform) to give 640 mg (overall yield: 55%) of Compound 21 as an amorphous substance. The obtained Compound 21 (2.00 g) was treated with a hydrogen chloride/methanol solution and then recrystallized from isopropanol to give 1.04 g of hydrochloride of Compound 21.

Provenance & Evidence