HRID80098

反应详情

EQUATION

反应方程式

HRID 80098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Sodium methoxide (225 mg, 4.165 mmol) was added dropwise to a stirred solution of 1-(2-chloro-pyridin-4-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (58A: 100 mg, 0.374 mmol) in 1,4-dioxane (20 mL) over a period of 10 minutes. The resulting mixture was heated to 110° C. and maintained at the same temperature for 4 days. The reaction was monitored by TLC (10% MeOH in CHCl3). The solvent was distilled from the reaction mixture and the concentrate was partitioned between water and ethylacetate. The organic layer was dried over Na2SO4 to afford the crude product. Purification by column preparative HPLC afforded 30 mg of the product (30.61% yield).

WORKUP

后处理

  1. temperaturemaintained at the same temperature for 4 days
  2. distillationThe solvent was distilled from the reaction mixture
  3. customthe concentrate was partitioned between water and ethylacetate
  4. dry with materialThe organic layer was dried over Na2SO4
  5. customto afford the crude product
  6. customPurification by column preparative HPLC