HRID2381377

反应详情

EQUATION

反应方程式

HRID 2381377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A solution of 3-cyclopentyl-2-(4-iodo-6-oxo-6H-pyridazin-1-yl)-propionic acid methyl ester (0.38 g, 1 mmol) in N,N-dimethylformamide (10 mL) was treated with 3-fluoro-pyridin-2-ol (0.15 g, 1 mmol) and potassium carbonate (0.16 g, 1.2 mmol). The reaction was heated at 120° C. for 4 h and then concentrated in vacuo. The residue was partitioned between water and methylene chloride. The aqueous layer was back extracted with methylene chloride. The combined organics were washed with a saturated aqueous sodium chloride solution, and then concentrated in vacuo. Chromatography (1/1 ethyl acetate/petroleum ether) afforded 3-cyclopentyl-2-[4-(3-fluoro-pyridin-2-yloxy)-6-oxo-6H-pyridazin-1-yl]-propionic acid methyl ester (0.19 g, 53%).

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. customThe residue was partitioned between water and methylene chloride
  3. extractionThe aqueous layer was back extracted with methylene chloride
  4. washThe combined organics were washed with a saturated aqueous sodium chloride solution
  5. concentrationconcentrated in vacuo