反应详情

To a suspension of sodium hydride (60% dispersion in mineral oil) (19.1 mg, 0.477 mmol) in anhydrous DMF (3.2 mL) was added solution of methyl 2-(2-(1H-tetrazol-1-yl)pyrimidin-5-yl)acetate (100 mg, 0.454 mmol) in anhydrous DMF (1.4 mL) at room temperature. Stirred for 10 min, then added methyl iodide (42.6 μl, 0.681 mmol) dropwise. Stirred at room temperature for 1 h. Reaction mixture was diluted with ethyl acetate and washed with water (3 times). Organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by MPLC, eluting with 20-100% ethyl acetate/hexanes, 26 column volumes. LC/MS: [(M+1)]+=235.2;

1. stirringStirred at room temperature for 1 h
2. customReaction mixture
3. washwashed with water (3 times)
4. washOrganic layer was washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customThe residue was purified by MPLC
8. washeluting with 20-100% ethyl acetate/hexanes, 26 column volumes