Hydrogen Peroxide → HCID 22475868, compound

Participants

Reaction Conditions

Reaction Steps

140.6 ml (0.225 mol, 1.6M) of butyllithium are added dropwise under nitrogen at 0° C. over the course of 30 minutes to a solution of 31.9 ml (0.225 mol) of diisopropylamine in 80 ml of tetrahydrofuran. This solution is added dropwise at -30° C. over the course of 90 minutes to a solution of 41.1 g (0.225 mol) of 2,4,6-trimethylbenzoyl chloride and 12 ml (0.102 mol) of isobutylphosphine in 200 ml of tetrahydrofuran. After the mixture has been stirred for 2 hours at -30° C., the yellow solution is allowed to warm to room temperature and is washed once with water. The organic phase is dried using magnesium sulfate, filtered and evaporated on a rotary evaporator. The residue is dissolved in 200 ml of toluene, and 11.6 g (0.102 mol) of 30% hydrogen peroxide are added. After the mixture has been stirred for 2 hours, it is washed first with water then with saturated sodium hydrogen carbonate solution. The organic phase is then dried using magnesium sulfate and filtered, and the solution is evaporated on a rotary evaporator. Crystallisation from hexane gives 27.8 g (68.5% of theory) of the abovementioned compound as a yellow powder. The melting point is 85°-86° C.

Provenance & Evidence