HRID2371800

反应详情

EQUATION

反应方程式

HRID 2371800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. washthe solution was washed (1N hydrochloric acid, brine)
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customThe residue was recrystallized from 21 ml of 1:0.5:1 methylene chloride
  5. dry with materialmethanol:hexane, ground to a powder and vacuum dried at 100° C.