HRID988284
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
A mixture of 6-methoxysalicylic acid (10.0 g, 59.5 mmol) in methanol (40 mL) and sulfuric acid (2 mL) is heated at reflux 48 h. Although some acid remains the reaction is concentrated to remove the methanol and partitioned between ethyl acetate and saturated sodium carbonate solution. The organic phase is separated and washed with sodium carbonate until no acid remains by TLC analysis. The organic phase is dried and concentrated to provide the title compound as a low melting solid.
WORKUP
后处理
- temperatureis heated
- temperatureat reflux 48 h
- concentrationis concentrated
- customto remove the methanol
- custompartitioned between ethyl acetate and saturated sodium carbonate solution
- customThe organic phase is separated
- washwashed with sodium carbonate until no acid
- customThe organic phase is dried
- concentrationconcentrated