反应详情

To a mixture of 5-formyl-2-{[3-(trifluoromethyl)phenyl]oxy}benzonitrile (1 g, 3.43 mmol) and dimethyl (1-diazo-2-oxopropyl)phosphonate (1.326 g, 6.87 mmol) in methanol (45 mL), was added potassium carbonate (2.373 g, 17.17 mmol) under argon. The reaction mixture was stirred for 1 h at rt, concentrated. The residue was dissolved in EtOAc (150 mL), washed with sat. ammonium hydrochloride solution (30 mL×3), water 30 mL, concentrated. Purification via ISCO system (EA/PE=1:20) afforded the title compound as a pale yellow oil. LC-MS (ESI): m/z 288 [M+H]+; 3.71 min (ret time).

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in EtOAc (150 mL)
3. washwashed with sat. ammonium hydrochloride solution (30 mL×3), water 30 mL
4. concentrationconcentrated
5. customPurification via ISCO system (EA/PE=1:20)