HRID333064

反应详情

EQUATION

反应方程式

HRID 333064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

(E)-4,4,5,5,5-Pentafluoro-N-[2-[[2-(2-methyl-1,3-dioxolan-2-yl)-4-pyridyl]amino]ethyl]pent-2-enamide (35 mg, 0.09 mmol) was dissolved in aceton (1 ml), 4M hydrochloric acid (0.5 ml) was added and the mixture was stirred in a closed vessel at 100° C. for 15 minutes with microwave heating. The mixture was diluted with water, extracted with ethyl acetate and the organic phase was washed with brine, dried over magnesium sulfate and evaporated to dryness. The resulting residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 2.5 mg (0.0071 mmol, 7.9%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washthe organic phase was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated to dryness
  5. customThe resulting residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)
  6. customto yield 2.5 mg (0.0071 mmol, 7.9%)