HRID421803

反应详情

EQUATION

反应方程式

HRID 421803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred solution of methyl 5-{[6-(4-cyanophenyl)-5-(cyclopropylcarbonyl)-4-methyl-2-oxo-3-[3-(trifluoromethyl)phenyl]-3,6-dihydropyrimidin-1(2H)-yl]methyl}-2-furoate (Example 42) (50 mg, 0.09 mmol) in tetrahydrofuran (1.5 ml) is treated with a solution of lithium hydroxide (2.34 mg, 0.1 mmol) in water (1.5 ml). After three hours stirring at room temperature, additional lithium hydroxide (2.34 mg, 0.1 mmol) is added. The reaction solution is stirred overnight (16 h), then allowed to stand for 48 h. The solution is acidified 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/water 30:70→90:10). The title compound is isolated as a brownish solid.

WORKUP

后处理

  1. stirringThe reaction solution is stirred overnight (16 h)
  2. waitto stand for 48 h
  3. stirringAfter 5 minutes stirring
  4. customa precipitate is obtained
  5. customthe crude reaction solution
  6. customis purified directly by preparative HPLC (RP18 column; eluent: acetonitrile/water 30:70→90:10)