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
In a similar manner to Step 1 of Example 347, isovanillic acid (5.00 g, 29.7 mmol) was suspended in dichloromethane (100 mL), and the suspension was treated with diisopropylethylamine (22.8 mL, 131 mmol) and chloromethyl methyl ether (4.96 mL, 65.4 mmol). The solvent was evaporated under reduced pressure. The residue was dissolved in methanol (50 mL) and treated with 4 mol/L aqueous potassium hydroxide solution (50 mL). The solvent was evaporated under reduced pressure. The residue was added with 4 mol/L hydrochloric acid. The precipitated solid was collected by filtration and washed with water, followed by drying under reduced pressure to obtain 3-methoxymethoxy-4-methoxybenzoic acid (4.82 g, yield 76%).
WORKUP
后处理
- customThe solvent was evaporated under reduced pressure
- dissolutionThe residue was dissolved in methanol (50 mL)
- additiontreated with 4 mol/L aqueous potassium hydroxide solution (50 mL)
- customThe solvent was evaporated under reduced pressure
- additionThe residue was added with 4 mol/L hydrochloric acid
- filtrationThe precipitated solid was collected by filtration
- washwashed with water
- customby drying under reduced pressure