HRID2381399

反应详情

EQUATION

反应方程式

HRID 2381399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A solution of 3-cyclopentyl-2-(4-hydroxy-6-oxo-6H-pyridazin-1-yl)-propionic acid methyl ester (3.0 g, 11.3 mmol) in N,N-dimethylformamide was treated with potassium carbonate (2.33 g, 16.9 mmol) and 2-chloro-4-trifluoromethyl-pyrimidine (3.1 g, 16.9 mmol). The reaction mixture was stirred at 110° C. for 1 h. At this time, the reaction was cooled to 25° C. and concentrated in vacuo. The residue was partitioned between water and ethyl acetate. The combined organics were washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered, and concentrated in vacuo. Chromatography afforded 3-cyclopentyl-2-[6-oxo-4-(4-trifluoromethyl-pyrimidin-2-yloxy)-6H-pyridazin-1-yl]-propionic acid methyl ester as a light oil (4.0 g, 86%).

WORKUP

后处理

  1. temperatureAt this time, the reaction was cooled to 25° C.
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between water and ethyl acetate
  4. washThe combined organics were washed with a saturated aqueous sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo