HRID2381492

反应详情

EQUATION

反应方程式

HRID 2381492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of 3-cyclopentyl-2-(6-oxo-6H-pyridazin-1-yl)-propionic acid methyl ester (2.99 g, 11.97 mmol) in methanol (7.9 mL, 1.5M) was treated with a 4N aqueous sodium hydroxide solution (3.29 mL, 13.16 mmol) and stirred at 25° C. overnight. At this time, the reaction was concentrated in vacuo. The residue was partitioned between water (100 mL) which was acidified with a 2N aqueous hydrochloric acid solution and a solution of 90/10 methylene chloride/methanol (3×75 mL). The combined organics were dried over sodium sulfate, filtered and concentrated in vacuo to afford 3-cyclopentyl-2-(6-oxo-6H-pyridazin-1-yl)-propionic acid (2.45 g, 86%) as a light pink solid; ES+-HRMS m/e calcd for C12H16N2O3 [M+H+] 237.1234, found 237.1233.

WORKUP

后处理

  1. concentrationAt this time, the reaction was concentrated in vacuo
  2. customThe residue was partitioned between water (100 mL) which
  3. dry with materialThe combined organics were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo