反应详情

To a stirred solution of Ethyl 2-(3-(2-chloro-6-methylbenzyloxy)phenyl)acetate (Step B, 4.94 g, 15.5 mmol) in absolute ethanol (80 ml) was added 1N NaOH (40 ml) at room temperature. The reaction mixture was stirred for 3 hours, acidified to pH 3.5-4.0 by adding 1N HCl and concentrated. The residue was taken into chloroform and washed with 0.1N HCl, brine, dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (chloroform:methanol, 95:5 spiked with acetic acid) to give the title compound.

1. concentrationconcentrated
2. washwashed with 0.1N HCl, brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified by flash chromatography on a silica gel column (chloroform:methanol, 95:5 spiked with acetic acid)