HRID1242059
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 a solution of 4-hydroxy-isobenzofuran-1,3-dione (0.5 g, 3.03 mmol) in anhydrous N,N-dimethylformamide (6 ml) under nitrogen was added diisopropylethylamine (1.05 ml, 6.06 mmol). The solution was stirred with cooling in an ice bath and chloromethyl methyl ether (0.46 ml, 6.06 mmol) was added. The reaction was allowed to slowly warm to ambient temperature and then stirred for an additional 7 h. The mixture was concentrated in vacuo to a small volume and diluted with ethyl acetate (75 ml). The organic layer was washed with water (2×40 ml), brine (20 ml), dried (Na2SO4), filtered, and the solvent evaporated in vacuo to give 0.6 g (95%) of 4-methoxymethoxy-isobenzofuran-1,3-dione as a solid.
WORKUP
后处理
- temperaturewith cooling in an ice bath
- stirringstirred for an additional 7 h
- concentrationThe mixture was concentrated in vacuo to a small volume
- additiondiluted with ethyl acetate (75 ml)
- washThe organic layer was washed with water (2×40 ml), brine (20 ml)
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customthe solvent evaporated in vacuo