反应详情

2.0 g (10.72 mmol) of 4-Chloro-3-hydroxy-benzoic acid methyl ester was dissolved in 20 ml of anhydrous tetrahydrofuran. To this solution was added 2.25 g (11.79 mmol) of 2-(2,4-Dichlorophenyl)-ethanol, 10.71 g (equivalent to 32.2 mmol PPh3) of triphenylphosphine derivatized polystyrene and 5.6 g (32.2 mmol) of DEAD. The solution was shaken for 16 h at RT. The polymer was filtered off and washed with ethyl acetate. The solvent was removed under reduced pressure. The residue was taken-up in ethyl acetate and the solution was washed three times with water and twice with saturated aqueous sodium chloride. The organic phase was dried with magnesium sulphate, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel eluting with ethyl acetate/n-heptane (1/6).

1. filtrationThe polymer was filtered off
2. washwashed with ethyl acetate
3. customThe solvent was removed under reduced pressure
4. washthe solution was washed three times with water
5. dry with materialThe organic phase was dried with magnesium sulphate
6. filtrationfiltered
7. customthe solvent was removed under reduced pressure
8. customThe residue was chromatographed on silica gel eluting with ethyl acetate/n-heptane (1/6)