HRID1915900

反应详情

EQUATION

反应方程式

HRID 1915900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

CuSO4 (with 5H2O, 65 mg) was added to a mixture of the above made 5-bromo-2-(2-fluorophenyl)pyrimidine-4-carboxylic acid (770 mg, 2.59 mmol) and 28% aqueous ammonium hydroxide (12 ml). The reaction was heated in a microwave reactor at 110° C. for 30 min. It was cooled to RT and concentrated in vacuo. The residue was diluted with 1N HCl (20 mL) and extracted with EtOAc 3×. Combined organic extracts were dried over sodium sulfate and filtered and concentrated to give 5-amino-2-(2-fluorophenyl)pyrimidine-4-carboxylic acid (320 mg, 53%).

WORKUP

后处理

  1. temperatureIt was cooled to RT
  2. concentrationconcentrated in vacuo
  3. additionThe residue was diluted with 1N HCl (20 mL)
  4. extractionextracted with EtOAc 3×
  5. dry with materialCombined organic extracts were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated