Ammonium Chloride → HCID 10683618, compound

Participants

Reaction Steps

0.15 g of nickel catalyst of expanded formula Ni(Acac)2 is added, in a 0.25 liter three-necked Erlenmeyer flask rendered inert with nitrogen, at a temperature below 5° C. and in one step, to the mixture in solution of 15 g (0.07 mol) of the compound of Example 8, 150 ml of tetrahydrofuran and 34.6 ml (0.07 mol) of a 2M solution of benzylmagnesium chloride in tetrahydrofuran. The medium is brought back to ambient temperature and, at the end of the progression of the coupling, treated by addition of 50 ml of a 10% ammonium chloride solution. The upper organic phase is separated, washed with an additional 50 ml of a 10% ammonium chloride solution and then washed with water. The organic phase is evaporated to dryness in order to obtain an oily residue (boiling temperature under 5 mbar=140-150° C.) which is purified again by chromatography on silica gel, elution being carried out with toluene, in order to result in 3.2 g of 2,4-dimethoxy-5-(1-methylethyl)-6-(phenylmethyl)pyrimidine.

Provenance & Evidence