反应详情

The fine suspension obtained by mixing 40 g (0.177 mol) of the compound of Example 2, 200 ml of toluene and 2 g of nickel catalyst NiCl2.dppe is brought to 0° C. in a 0.5 liter reactor, rendered inert with nitrogen and equipped with an anchor stirrer, and treated by addition of 97.6 ml (0.195 mol) of a 2M solution of benzylmagnesium chloride in tetrahydrofuran without exceeding 10° C. At the end of the progression of the coupling, the reaction mixture is treated by addition of 120 ml of a 10% ammonium chloride solution and the upper organic phase is separated, washed with 10% aqueous ammonium chloride solution until decoloured and evaporated to dryness under vacuum. The oily residue obtained is purified by distillation under vacuum in order to remove, as distillation tops, the residual starting material and to result in 39.6 g of 2,4-dichloro-5-(1-methylethyl)-6-(phenylmethyl)pyrimidine (yellow oil, boiling temperature at 0.2 mbar=145-150° C.).

1. customThe fine suspension obtained
2. customequipped with an anchor stirrer
3. customwithout exceeding 10° C
4. customthe upper organic phase is separated
5. washwashed with 10% aqueous ammonium chloride solution
6. customevaporated to dryness under vacuum
7. customThe oily residue obtained
8. distillationis purified by distillation under vacuum in order
9. customto remove, as distillation tops
10. customto result in 39.6 g of 2,4-dichloro-5-(1-methylethyl)-6-(phenylmethyl)pyrimidine (yellow oil, boiling temperature at 0.2 mbar=145-150° C.)