HRID421804

反应详情

EQUATION

反应方程式

HRID 421804 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of methyl 2-{[6-(4-cyanophenyl)-5-(cyclopropylcarbonyl)-4-methyl-2-oxo-3-[3-(trifluoromethyl)phenyl]-3,6-dihydropyrimidin-1(2H)-yl]methyl}-1,3-oxazole-4-carboxylate (Example 43) (50 mg, 0.09 mmol) in tetrahydrofuran (1.5 ml) is added a solution of lithium hydroxide (4.24 mg, 0.18 mmol) in water (1.5 ml). The reaction solution is stirred at room temperature overnight (16 h). The pH of the solution is adjusted to less than pH 7 with 1 N hydrochloric acid (500 μl). After 5 minutes stirring, a precipitate is obtained. Methanol (3 ml) is added, and the crude reaction solution is purified directly by preparative HPLC (RP18 column; eluent: acetonitrile/0.1% aq. formic acid 30:70→90:10). The title compound is isolated as a colourless solid.

WORKUP

后处理

  1. stirringAfter 5 minutes stirring
  2. customa precipitate is obtained
  3. customthe crude reaction solution
  4. customis purified directly by preparative HPLC (RP18 column; eluent: acetonitrile/0.1% aq. formic acid 30:70→90:10)