反应详情

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.

1. temperatureThe mixture was heated
2. temperatureunder reflux
3. dissolutionwas completely dissolved
4. temperatureunder reflux
5. filtrationthe precipitated crystals were collected by filtration
6. washThe crystals were sequentially washed with 2-propanol (50 mL×3) and tert-butyl methyl ether (50 mL×3)
7. customdried under reduced pressure