Hydrochloric Acid → HCID 13091039, compound

Participants

Reaction Steps

The substance [20] (74.4 g, 85.4 mM) was dissolved in methanol (300 ml), and 1 N NaOH (110 ml, 1.3 molar excess) was added dropwise at 0° C., and the mixture was stirred at room temperature for three hours. After neutralizing at 0° C. by adding 1 N HCl (26 ml), the methanol was distilled off in vacuo. The aqueous layer was washed twice with ether, 1 N HCl (86 ml) was added at 0° C. and then was extracted with ethyl acetate. The ethyl acetate layer was washed twice with water, dried with anhydrous magnesium sulfate and concentrated in vacuo. Hexane was added to the residue and the thus-formed precipitate was filtered. The precipitate was dissolved in a small amount of chloroform and charged on a column of silica gel packed with chloroform. Elution was carried out with chloroform, chloroform-ethyl acetate (1:1) and chloroform-ethanol-ethyl acetate (5:1:5). The fractions corresponding to the substance as checked by TLC were collected and dried in vacuo to obtain the substance [21] (53.75 g, yield: 81%).

Provenance & Evidence