反应详情

To a solution of 2-(2-methoxy-vinyl)-6-nitro-benzoic acid methyl ester (Step A, 3.33 g, 14.1 mmol, 1.0 eq) and CH3CN (20 mL) was added NaI (2.3 g, 15.5 mmol, 1.1 eq) and TMSCl (2 mL, 15.5 mmol, 1.1 eq). The reaction was stirred at RT for 4 h, then quenched with saturated NH4Cl and extracted with EtOAc. The organic layer was washed with H2O and brine, dried (MgSO4) and concentrated in vacuo to give a red-orange oil. Purification by silica flash chromatography (0-30% EtOAc:hexane) gave the desired compound as an orange oil.

1. customquenched with saturated NH4Cl
2. extractionextracted with EtOAc
3. washThe organic layer was washed with H2O and brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give a red-orange oil
7. customPurification by silica flash chromatography (0-30% EtOAc:hexane)