Dichloromethane → HCID 67372107, compound

Participants

Reaction Steps

To a solution of the compound (150 mg) obtained in Example 44 in a mixture of anhydrous tetrahydrofuran (8 mL) and anhydrous dichloromethane (8 mL) was added 90% potassium trimethylsilanolate (125 mg) at room temperature, followed by stirring at the same temperature under nitrogen atmosphere for four hours. Insoluble matter was collected by filtration, was washed with dichloromethane and was dried. The insoluble matter was dissolved in water (1 mL) and was then treated with 1 N hydrochloric acid to adjust the pH of the mixture to 5 to 5.6. The precipitate was collected by filtration, washed with water and dried. The precipitate was suspended in methanol, and mixed with 10% solution of hydrogen chloride in methanol, then the mixture was stirred at room temperature, and the solvent was removed under reduced pressure. The residue was suspended in acetonitrile, washed at 40 to 50° C. with stirring for one hour, was collected by filtration, and dried under reduced pressure to yield the titled compound (58 mg) as crystals.

Provenance & Evidence