反应详情

A solution of (5-{(1R)2-[bis(phenylmethyl)amino]-1-hydroxyethyl}-2-hydroxyphenyl)formamide (354 mg) in DMF (10 ml) under nitrogen was treated with sodium hydride (60% dispersion in mineral oil, 38 mg) and the mixture stirred at 20° for 10 min. 2-(Trimethylsilyl)ethoxymethyl chloride (0.17 ml) was added and the mixture was stirred at 20° for 3 h. Phosphate buffer solution (pH 6.5) and water were added and the mixture was extracted with EtOAc. The extract was washed with water and dried (Na2SO4). Solvent evaporation in vacuo gave a residue which was purified on a silica SPE bond elut cartridge (20 g) using a gradient of 0% to 2% MeOH in DCM (Gradmaster™). The appropriate fractions were evaporated in vacuo to give the title compound (286 mg). LCMS RT=3.08 min.

1. stirringthe mixture was stirred at 20° for 3 h
2. extractionthe mixture was extracted with EtOAc
3. washThe extract was washed with water
4. dry with materialdried (Na2SO4)
5. customSolvent evaporation in vacuo
6. customgave a residue which
7. customwas purified on a silica SPE bond elut cartridge (20 g)
8. customThe appropriate fractions were evaporated in vacuo