Sodium Hydroxide → HCID 131732142, compound

Participants

Reaction Conditions

Reaction Steps

To a aqueous solution of NH2OH.HCl (8.4 g, 121.2 mmol) and NaOH (2.2 g, 19.54 mmol) in H2O (20 mL) was added a solution of Example 48C (2.81 g, 8.36 mmol) in MeOH (70 mL) and the mixture was heated at 65° C. for 8 hours. The mixture was cooled to room temperature, sufficient water was added and MeOH was removed under reduced pressure. The resulting slurry was adjusted to pH=10 with NaOH solution (2.5 N) and extracted with dichloromethane. The combined organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated to give a crude product, which was purified by column chromatography (SiO2, dichloromethane:MeOH from 100:1 to 10:1) to get the title compound.

Provenance & Evidence