Hydrochloric Acid → M-58996

Participants

Reaction Steps

The compound (22.0 g) obtained in Example 1 was suspended in a mixture of ethanol (264 mL) and water (176 mL). The mixture was heated under reflux and was completely dissolved by adding 1 N hydrochloric acid (58.7 mL) dropwise while keeping the mixture under reflux. After cooling to room temperature, the precipitated crystals were collected by filtration. The crystals were sequentially washed with 2-propanol (50 mL×3) and tert-butyl methyl ether (50 mL×3), dried under reduced pressure to yield the titled compound (21.1 g) as crystals. Elementary analysis revealed that the compound is monohydrate.

Provenance & Evidence