HRID398210
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 55 °C
PROCEDURE
实验过程
A mixture of 4-benzyloxy-2-propylphenol (3.89 mmol), toluene-4-sulfonic acid 2-(5-methyl-2-biphenyl-4-yl-oxazol-4-ly) ethyl ester (4.67 mmol) (see Ex. 1, part F) and cesium carbonate (1.65 g 5.06 mmol) in anhydrous DMF (8 mL) was heated for 18 h at 55° C. The mixture was concentrated in vacuo, and the residue was partitioned between ethyl acetate (100 mL) and water (50 mL), washed with brine (50 mL), dried (Na2SO4), and removed in vacuo to give a crude oil which was purified using the Biotage FlashElute chromatography system using a 40 L normal phase cartridge, eluting with 10-15% ethyl acetate/hexanes to give 4-[2-(4-benzyloxy-3-propylphenoxy)ethyl]-5-methyl-2-phenyloxazole.
WORKUP
后处理
- concentrationThe mixture was concentrated in vacuo
- customthe residue was partitioned between ethyl acetate (100 mL) and water (50 mL)
- washwashed with brine (50 mL)
- dry with materialdried (Na2SO4)
- customremoved in vacuo
- customto give a crude oil which
- customwas purified
- washeluting with 10-15% ethyl acetate/hexanes