HRID2381507

反应详情

EQUATION

反应方程式

HRID 2381507 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-3-phenoxy-6H-pyridazin-1-yl)-propionic acid methyl ester (1.03 g, 3.03 mmol) in methanol (8.5 mL, 0.36M) was treated with a 4N aqueous sodium hydroxide solution (0.83 mL, 3.34 mmol) and stirred at 25° C. overnight. After this time, the reaction was concentrated in vacuo. The residue was diluted with water (100 mL) and acidified to pH=1 with a 3N aqueous hydrochloric acid solution. The resulting solids were collected by filtration, rinsed with water, air dried and then further dried in vacuo to afford 3-cyclopentyl-2-(6-oxo-3-phenoxy-6H-pyridazin-1-yl)-propionic acid (0.81 g, 81%) as a white solid. 1H-NMR (300 MHz, DMSO-d6) δ ppm 0.94 (br s, 2H), 1.29-1.70 (m, 7H), 1.79 (br s, 1H), 1.85-2.05 (m, 1H), 5.08 (dd, J=10.6, 3.0 Hz, 1H), 7.06 (d, J=9.7 Hz, 1H), 7.10-7.25 (m, 3H), 7.34-7.45 (m, 3H).

WORKUP

后处理

  1. concentrationAfter this time, the reaction was concentrated in vacuo
  2. additionThe residue was diluted with water (100 mL)
  3. filtrationThe resulting solids were collected by filtration
  4. washrinsed with water, air
  5. customdried
  6. customfurther dried in vacuo