HRID2070874
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
2-(2,4-Dimethoxybenzyl)-5-nitroisoindolin-1-one. A mixture of methyl 2-(bromomethyl)-4-nitrobenzoate (2.5 g, 9.12 mmol), (2,4-dimethoxyphenyl)methanamine (1.525 g, 9.12 mmol), triethylamine (3.81 mL, 27.4 mmol) in methanol (25 mL) was refluxed for 16 h. The mixture was diluted with ethyl acetate, washed with dilute hydrochloric acid and brine, dried over magnesium sulfate, filtered, and concentrated on a rotary evaporator to dryness. Flash chromatography (30-50% ethyl acetate in hexane) gave the desired product as a yellow solid (2.5 g, 7.68 mmol, 84% yield). MS (ESI) m/z 329.9 [M+1]+.
WORKUP
后处理
- temperaturewas refluxed for 16 h
- washwashed with dilute hydrochloric acid and brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated on a rotary evaporator to dryness