HRID29423
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 5-formyl-4-hydroxy-3-methyl-benzofuran-2-carboxylic acid tert-butyl ester (430 mg, 1.56 mmol) was added 8 mL of THF, and sodium cyanoborohydride (117 mg, 1.87 mmol) was added in one portion. The solution was stirred at room temperature for 1 h and then placed in a 65° C. oil bath overnight. The solvent was removed under vacuum and water was added. The mixture was extracted with ethyl acetate. Removal of the solvent gave the crude product, which was purified by column chromatography to give 70 mg of 4-hydroxy-3,5-dimethyl-benzofuran-2-carboxylic acid tert-butyl ester as a white solid.
WORKUP
后处理
- additionwas added in one portion
- customplaced in a 65° C.
- customovernight
- customThe solvent was removed under vacuum and water
- additionwas added
- extractionThe mixture was extracted with ethyl acetate
- customRemoval of the solvent
- customgave the crude product, which
- customwas purified by column chromatography