Hydrogen Peroxide → HCID 131730705, compound

Participants

Reaction Steps

100 g Chimassorb 2020® (commercial product of Ciba Specialty Chemicals Inc.) in t-butanol is reacted with 120 g 50% hydrogen peroxide in the presence of 3 g sodium carbonate decahydrate to afford the Chimassorb 2020-nitroxyl after approximately 7-9 hrs. of reaction at 75° C. The batch is treated with sodium sulfite solution to destroy unreacted peroxides and then the aqueous layer is split off. The batch pH is brought to 7 with a trace of glacial acetic acid. Additional 140 g t-butanol is added, followed by 100 g butyraldehyde and 0.2 g Cu(I)Cl. Hydrogen peroxide (120 g) is dosed in while maintaining the reaction temperature at 35° C. The batch is on hold at 35° C. until the reaction is complete. A combination of sodium sulfite and sodium hydroxide solution is added. t-Butanol/water is stripped off under partial vacuum (15-20 mm Hg.) and the t-butanol is replaced by hexane. After 30 min. of stirring at 60° C., the aqueous layer is split. The batch pH is adjusted to 7 with a small quantity of acid. An EDTA wash is performed and the product is isolated with hot water stripping and dried in an oven at 80° C. to constant weight. Yield: 117 g; yellow powder.

Provenance & Evidence