反应详情

Trimethylsulfoxonium iodide (14.15 g, 63 mmol) is suspended in dry dimethylsulfoxide (126 mL) and sodium hydride (60% in mineral oil, 2.52 g, 63 mmol) is added. The mixture is stirred for 40 minutes and then a solution of 4-methoxycinnamic acid ethyl ester (5 g, 24.2 mmol) in dry dimethylsulfoxide (64 mL) is added and the mixture stirred for 3 hours at room temperature. The mixture is diluted with water and extracted with ethyl acetate, the organic phase is dried by passing through a phase separator and the solvent is removed under vacuum. The residue is purified by flash chromatography (10% ethyl acetate in cyclohexane) to give the title compound (yield 1.43 g). LC (METHOD 11): tR=7.74 min; Mass spectrum (ESI+): m/z=221 [M+H]+.

1. stirringthe mixture stirred for 3 hours at room temperature
2. extractionextracted with ethyl acetate
3. customthe organic phase is dried
4. customthe solvent is removed under vacuum
5. customThe residue is purified by flash chromatography (10% ethyl acetate in cyclohexane)