Sodium Hydroxide → HCID 89823605, compound

Participants

Reaction Conditions

Reaction Steps

To an aqueous solution of hydroxylamine hydrochloride (458 g, 6.59 mol) and sodium hydroxide (120 g, 3 mol) in water (350 mL) was added a solution of Example 1D (119 g, 0.454 mol) in methanol (2 L) and the mixture was stirred at 65° C. for 8 hours. The mixture was cooled to room temperature, sufficient water was added and the methanol was removed under reduced pressure. The resulting slurry was adjusted to pH 10 with an aqueous sodium hydroxide solution (2.5 N) and the reaction mixture was extracted with dichloromethane. The combined organic fractions were washed with brine, dried over sodium sulfate, filtered, and concentrated to afford the title compound, which was used in the next step without further purification.

Provenance & Evidence