反应详情

5-(Adamantan-1-yloxymethyl)-2-cyclohexyl-2H-pyrazol-3-ol (0.29 g, 0.88 mmol) and sodium hydride (50 mg, 1.25 mmol of a 40% suspension in mineral oil) were stirred in THF-DMF (1:1) (10 mL) at 0° C. for 0.5 h, then allowed to warm to room temperature. Dimethyl sulphate (0.1 mL, 1 mmol) was added and the mixture stirred overnight. After concentration in vacuo, the mixture was poured into water (10 mL) and extracted with EtOAc (20 mL). The organic layer was separated washed with water (2×10 mL) and dried (MgSO4). Filtration and evaporation of the solvent afforded a yellow oil, which was purified by chromatography with EtOAc-hexane (1:1) as eluant. (0.24 g, 81%).

1. concentrationAfter concentration in vacuo
2. additionthe mixture was poured into water (10 mL)
3. extractionextracted with EtOAc (20 mL)
4. customThe organic layer was separated
5. washwashed with water (2×10 mL)
6. dry with materialdried (MgSO4)
7. filtrationFiltration and evaporation of the solvent
8. customafforded a yellow oil, which
9. customwas purified by chromatography with EtOAc-hexane (1:1) as eluant