HRID1756449

反应详情

EQUATION

反应方程式

HRID 1756449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6 g (0.15 mol) of sodium hydroxide are added to a solution of 6.08 g (14 mmol) of methyl 4-[3-(1-adamantyl) -4-methoxyphenylureido]benzoate in 75 ml of methanol and the mixture is stirred at room temperature for 3 hours and then heated to reflux for 3.5 hours. The reaction mixture is evaporated, the residue is then taken up with 100 ml of water and the mixture is acidified to pH 1. The solid is filtered off, rinsed with water, dried and recrystallized in a tetrahydrofuran/hexane mixture to yield 2.78 g (87% ) of 4-[3-(1-adamantyl)-4-methoxyphenylureido]benzoic acid, melting point 279°-282° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 3.5 hours
  3. customThe reaction mixture is evaporated
  4. filtrationThe solid is filtered off
  5. washrinsed with water
  6. customdried
  7. customrecrystallized in a tetrahydrofuran/hexane mixture