反应详情

温度

0 °C

Methanesulfonylchloride (3.3 mL) was added dropwise over 5 min to a solution of 4-(2-hydroxyethoxy)benzaldehyde (example 108, step a) (6.4 g) and triethylamine (6.4 mL) in DCM (30 mL) at 0° C. under argon. The resulting mixture was stirred at 0° C. for 10 min and then at RT for 1 h. The reaction mixture was washed with brine (2×30 mL), dried over sodium sulphate, filtered and evaporated in vacuo. The residue was purified by silica gel chromatography eluting with 40-50% EtOAc in petroleum ether (40-60° C.) to give the subtitled compound as a viscous yellow oil. Yield 8.87 g.

1. waitat RT for 1 h
2. washThe reaction mixture was washed with brine (2×30 mL)
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customevaporated in vacuo
6. customThe residue was purified by silica gel chromatography
7. washeluting with 40-50% EtOAc in petroleum ether (40-60° C.)