HRID2401472
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
- 80 °C
PROCEDURE
实验过程
To a solution of methyl 3-methoxy-2-methyl-4-nitrobenzoate (800 mg, 3.6 mmol) in CH3CN (10 mL) was added NBS (770 mg, 4.3 mmol) and AIBN (12 mg, 0.072 mmol) under the protection of N2. The mixture was refluxed at 80° C. for overnight. After the solvent was evaporated in vacuo, the resulting residue was purified by silica gel-column (eluting with PE/EA=15:1) to afford methyl 2-(bromomethyl)-3-methoxy-4-nitrobenzoate as yellow oil (910 mg, yield 84%). m/z (ES+APCI)+: [M−Br]+224.1.
WORKUP
后处理
- customAfter the solvent was evaporated in vacuo
- customthe resulting residue was purified by silica gel-column (eluting with PE/EA=15:1)