HRID927002

反应详情

EQUATION

反应方程式

HRID 927002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[5-Acetyl-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidin-4-yl]-5-cyano-benzoic acid methyl ester (intermediate 5)(612 mg, 1.30 mmol) and lithium hydroxide (93.3 mg, 3.90 mmol) are stirred in 1,4-dioxane (12.0 ml) and water (6.0 mL) at room temperature for 20 min Water (200 mL) is added and the mixture is acidified with hydrochloric acid (1.0 M, 44 mL) to a pH value of 3. The aqueous phase is extracted with ethyl acetate. The organic phase is washed twice with water, dried over MgSO4 and concentrated. Yield: 665 mg. ESI mass spectrum: [M+H]+=472; Retention time HPLC: 1.09 min (HPLC method Z018_S04).

WORKUP

后处理

  1. extractionThe aqueous phase is extracted with ethyl acetate
  2. washThe organic phase is washed twice with water
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. custom1.09 min (HPLC method Z018_S04)