HRID488485
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 solution of 2-{4-[2-(3,4-dichloro-phenyl)-ethyl]phenylamino}-5-nitrobenzoic acid methyl ester (340 mg, 0.76 mmol) and 1N NaOH (aq.) (4.0 mL) in EtOH (4.0 mL) and THF (4.0 mL) was heated to reflux for 16 hours. The solvent was removed in vacuum. The residue was diluted with H2O and acidified with concentrated HCl to pH 1. The mixture was then extracted with methylene chloride, dried (Na2SO4), filtered and concentrated in vacuo to yield a yellow solid, 329 mg (0.76 mmol, 100%) of the desired product mp 214-217° C.
WORKUP
后处理
- temperatureto reflux for 16 hours
- customThe solvent was removed in vacuum
- additionThe residue was diluted with H2O
- extractionThe mixture was then extracted with methylene chloride
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo