HRID333959

反应详情

EQUATION

反应方程式

HRID 333959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(E)-4-Ethyl-hex-2-enoic acid (21.3 mg, 0.15 mmol) was dissolved in DMF (350 μl), diisopropylethylamine was added (26 μl, 0.15 mmol) followed by HATU (57 mg, 0.15 mmol dissolved in 0.25 ml DMF). The mixture was stirred at room temperature for 15 minutes, then 2-methyl-4-piperazin-1-yl-7-(trifluoromethyl)quinoline (44 mg, 0.15 mmol, dissolved in 1 ml DMF) was added and stirring was continued overnight. The mixture was evaporated under reduced pressure, the residue was dissolved in dichloromethane, the solution was washed with 5% sodium bicarbonate solution and water, evaporated to dryness under reduced pressure. The residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 20.3 mg (0.48 mmol, 32.3%) of a solid.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued overnight
  3. customThe mixture was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in dichloromethane
  5. washthe solution was washed with 5% sodium bicarbonate solution and water
  6. customevaporated to dryness under reduced pressure
  7. customThe residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)