反应详情

To a stirred solution of Ethyl 3-hydroxybenzoate (12.21 g, 73.47 mmol) and triphenylphosphine (21.01 g, 80.13 mmol) in dry THF (100 ml) was added dropwise a solution of 2,6-Dimethylbenzyl alcohol (10 g, 73.5 mmol) and diisopropyl azodicarboxylate (16.19 g, 80.13 mmol) in dry THF (35 ml) and dry DMF (15 ml) at ambient temperature. After three hours of stirring at room temperature, the reaction mixture was diluted with diethyl ether and washed twice with water and brine. The combined organic layer was dried over Na2SO4, filtered, concentrated and purified by flash chromatography using ethyl acetate:hexane (1:3) as elutent.

1. washwashed twice with water and brine
2. dry with materialThe combined organic layer was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. custompurified by flash chromatography