Hydrogen Peroxide → HCID 22475868, compound

Participants

Reaction Conditions

Reaction Steps

140.6 ml (0.225 mol; 1.6M) of butyllithium are added dropwise over 30 minutes under nitrogen at 0° C. 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 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 (2-methylprop-1-yl)phosphine in 200 ml of tetrahydrofuran. After stirring for 2 h at -30° C., the yellow solution is warmed to room temperature and washed once with water. The organic phase is dried over magnesium sulfate, filtered, and the filtrate is concentrated 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 to the solution. The mixture is stirred for 2 h and washed first with water and then with a saturated solution of sodium hydrogencarbonate and afterwards dried over magnesium sulfate and filtered. The solution is concentrated on a rotary evaporator. Crystallisation of the residue from hexane gives 27.8 g (68.5% of theory) of the above compound as a yellow powder with a melting point of 85°-86 ° C.

Provenance & Evidence