HRID2245285
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2-Acetylamino-3-(2-[1,3]dioxan-2-yl-3-fluoro-phenyl)-acrylic acid methyl ester (10.6 g, 32.8 mmol) and pyridinium para-toluene sulfonate (2.06 g, 8.2 mmol) are heated to reflux for 20 hours in an acetone/water (120 ml/15 ml) mixture. The solvents are removed by evaporation and the aqueous residue is extracted with ethylacetate. The organic layer is washed with brine and dried over MgSO4 and evaporated. The crude product is recrystallised from ethylacetate/ether to afford 5.1 g of the desired compound. MS (ES+): m/e=206.2 (MH+)
WORKUP
后处理
- customThe solvents are removed by evaporation
- extractionthe aqueous residue is extracted with ethylacetate
- washThe organic layer is washed with brine
- dry with materialdried over MgSO4
- customevaporated
- customThe crude product is recrystallised from ethylacetate/ether