Hydrogen Peroxide → HCID 68851729, compound

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Reaction Steps

200 ml (0.332 mol; 1.6M) of butyllithium are added dropwise at 0° C., under argon, in the course of 30 minutes to a solution of 33.6 g (0.332 mol) of diisopropylamine in 100 ml of tetrahydrofuran. The resulting solution is added dropwise at −20° C. in the course of 2 hours to a solution of 60.6 g (0.332 mol) of 2,4,6-trimethylbenzoyl chloride and 36.4 g (0.151 mol) of 4-[bis(2-methoxy-ethyl)amino]-phenyl-phosphine (prepared as described in Example 1) in 200 ml of tetrahydrofuran. After 2 hours' stirring, the yellow reaction solution is heated to room temperature and the solvent is removed using a rotary evaporator. The residue is taken up in 200 ml of toluene and washed once with water. 17.1 g (0.151 mol; 30%) of hydrogen peroxide are added to the organic phase. After 2 hours' stirring, washing is carried out first with water, then with saturated sodium hydrogen carbonate solution. Drying is then carried out with magnesium sulfate, followed by filtration and concentration using a rotary evaporator. After crystallisation from isopropanol, 30.2 g (36.4% of theory) of the title compound are obtained in the form of a yellow powder having a melting point of 103–106° C. (31P-NMR 10.23 ppm).

Provenance & Evidence