HRID1929382

反应详情

EQUATION

反应方程式

HRID 1929382 的结构方程式

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A mixture of (2-amino-5-bromopyridin-3-yl)(6-fluoropyridin-2-yl)methanone (190 mg, 0.64 mmol), 1-Boc-homopiperazine (0.14 ml, 0.70 mmol) and potassium carbonate (310 mg, 2.24 mmol) in dimethylfonmamide (4 ml) was heated at 95° C. for 48 hours. The reaction mixture was cooled down to room temperature and concentrated in vacuo. The residue was slurried in EtOAc and K2CO3 was filtered off. The mother liquors were concentrated in vacuo. The resulting residue was purified on silica gel by flash column chromatography (ISCO Companion|, 12 g column, 0-20% EtOAc/Petrol) to give the title compound as a yellow solid (180 mg, 59% yield).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled down to room temperature
  2. concentrationconcentrated in vacuo
  3. filtrationK2CO3 was filtered off
  4. concentrationThe mother liquors were concentrated in vacuo
  5. customThe resulting residue was purified on silica gel by flash column chromatography (ISCO Companion|, 12 g column, 0-20% EtOAc/Petrol)