1,4-Dioxane hydrochloride → HCID 86650788, compound

Participants

Reaction Steps

The compound (3.62 g, 5.80 mmol) obtained in step A was dissolved in dichloromethane (12 ml), 4N hydrochloric acid-dioxane solution (12 ml) was added, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with chloroform, and the organic layer was washed with 1N aqueous sodium hydroxide solution, and dried over sodium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure. The obtained oil was dissolved in diethyl ether (58 ml), and 4N hydrochloric acid-ethyl acetate (3.14 ml, 12.6 mmol) was added to allow precipitation of a solid. This was collected by filtration, washed with diethyl ether, and dried under reduced pressure to give the title compound (2.96 g, yield 86%) as a pale-yellow solid.

Provenance & Evidence