HRID1528167
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of methylamine (2 M in methanol) at 0° C. was added dropwise to a solution of 14.82 g of ethyl 2-bromomethyl-6-methoxybenzoate in methanol and the reaction medium was stirred for 5 hours at 0° C. and left to stir at ambient temperature for 2 days. The solvent was evaporated off and 30 ml of a saturated sodium hydrogen carbonate solution were added to the residue. The product was extracted with ethyl acetate (3×50 ml). The organic phases were combined, dried over magnesium sulfate and evaporated. The residue was purified by chromatography on silica gel. 4.52 g of 7-methoxy-2-methyl-2,3-dihydroisoindol-1-one were obtained. Yield=47%.
WORKUP
后处理
- waitleft
- stirringto stir at ambient temperature for 2 days
- customThe solvent was evaporated off
- addition30 ml of a saturated sodium hydrogen carbonate solution were added to the residue
- extractionThe product was extracted with ethyl acetate (3×50 ml)
- dry with materialdried over magnesium sulfate
- customevaporated
- customThe residue was purified by chromatography on silica gel