HRID2371800
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 4-[7-(2-ethylbutylcarbamoyl)naphth-1-ylmethyl]-3-methoxybenzoic acid (189 mg), 4-dimethylaminopyridine (110 mg), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (172 mg), and o-toluenesulfonamide (96 mg) in methylene chloride (2 ml) was stirred for 18 h. Methylene chloride (25 ml) was added, and the solution was washed (1N hydrochloric acid, brine), dried (MgSO4) and evaporated. The residue was recrystallized from 21 ml of 1:0.5:1 methylene chloride:methanol:hexane, ground to a powder and vacuum dried at 100° C. to give the title compound (179 mg, 70%) as a colorless solid; mp 126.0°-128.0° C.
WORKUP
后处理
- washthe solution was washed (1N hydrochloric acid, brine)
- dry with materialdried (MgSO4)
- customevaporated
- customThe residue was recrystallized from 21 ml of 1:0.5:1 methylene chloride
- dry with materialmethanol:hexane, ground to a powder and vacuum dried at 100° C.