Hydrochloric Acid → HCID 59536813, compound

Participants

Reaction Steps

Of the compound from Example 163A, 11.3 g (33.98 mmol) were taken up in 61 ml (183.47 mmol) of 3M aqueous sodium hydroxide solution and heated under reflux for 36 h. The batch was then cooled, the fine precipitate was removed by filtration, and the filtrate was admixed, with ice cooling, with 28 ml (169.88 mmol) of half-concentrated hydrochloric acid to a pH of 10. The batch was filtered with suction and the product was dissolved out of the precipitate using methanol. The methanol was removed on a rotary evaporator. The residue was dried in an HV. This gave 9.78 g (69% of theory) of the title compound in 75% purity.

Provenance & Evidence