HRID2352871

反应详情

EQUATION

反应方程式

HRID 2352871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A small screw cap test tube was charged with 2,5-Dimethyl-2H-pyrazole-3-carboxylic acid [3-(3-hydroxymethylene-2-oxo-2,3-dihydro-1H-indole-6-carbonyl)-phenyl]-amide (as prepared in Example 60, 100 mg, 0.249 mmol) and THF (2 mL). To the resulting solution was added (4-Amino-phenyl)-acetic acid (41.4 mg, 0.274 mmol), and the mixture was stirred for 24 h at 65° C. Subsequently, the reaction mixture was cooled to room temperature. EtOAc (3 mL) was added to the mixture and was washed with 5% HCl(aq) (2 mL) and H2O (2×2 mL). The organic layers were combined dried over anhydrous Na2SO4, filtered and concentrated in vacuo The solid was then recrystallized from EtOAc/Hexanes affording 51% (0.068 g, 0.127 mmol) of the title compound.

WORKUP

后处理

  1. customA small screw cap test tube
  2. temperatureSubsequently, the reaction mixture was cooled to room temperature
  3. washwas washed with 5% HCl(aq) (2 mL) and H2O (2×2 mL)
  4. dry with materialThe organic layers were combined dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo The solid