反应详情

The above prepared 2-hydroxy-4-methoxy-5-methyl-benzaldehyde (1.97 g, 11.86 mmol) was dissolved in 30 mL of abs. THF and treated at −15° C. with iPrMgCl (14.8 mL of 2M [THF], 2.5 eq.) and the mixture kept at this temperature for 0.5 h. Careful pouring onto crashed ice/NH4Cl, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents left 2.45 g of the title compound as white crystals, almost perfectly pure according to TLC and NMR.

1. dissolutionwas dissolved in 30 mL of abs
2. additionCareful pouring
3. extractionice/NH4Cl, twofold extraction with AcOEt
4. washwashing with water and brine
5. dry with materialdrying over magnesium sulfate, and evaporation of the solvents
6. waitleft 2.45 g of the title compound as white crystals