HRID585299
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
2,6-naphthalenedicarboxylic acid dimethyl ester (26.0 g, 106 mmol) was dissolved in N,N-dimethylformamide (500 ml), and a 1N aqueous sodium hydroxide solution (106 ml) was added dropwise thereto at 100° C. over 30 minutes. After stirred for 3 hours, the solvent was distilled off under reduced pressure, water was added to the residue and the insolubles were filtered off. Concentrated hydrochloric acid (9 ml) was added to the filtrate, the precipitated crude product was filtered, washed with water, and recrystallized from hot methanol to obtain 6-(methoxycarbonyl)-2-naphthalenecarboxylic acid (14.6 g) as a white powder.
WORKUP
后处理
- distillationthe solvent was distilled off under reduced pressure, water
- additionwas added to the residue
- filtrationthe insolubles were filtered off
- additionConcentrated hydrochloric acid (9 ml) was added to the filtrate
- customthe precipitated crude product
- filtrationwas filtered
- washwashed with water
- customrecrystallized from hot methanol