HRID1052371

反应详情

EQUATION

反应方程式

HRID 1052371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Phenol (6 mg, 0.06 mmol) was dissolved in 450 μl of N,N-dimethylformamide. Potassium carbonate (6 mg, 0.05 mmol) was added and the reaction was stirred at room temperature for 30 min. (S)-tert-Butyl (3-bromo-1-(4-oxo-3-phenyl-3,4-dihydropyrrolo[2,1-f][1,2,4]triazin-2-yl)propyl)carbamate (45 mg, 0.03 mmol) and potassium iodide (1 mg, 0.001 mmol) were added and the reaction was heated at 70° C. for 3 h. The mixture was poured into a 4% aqueous sodium bicarbonate and extracted with ethyl acetate. The combined organic phases were washed with water, brine, dried over sodium sulphate and evaporated under reduced pressure. The crude was purified by SP1® Purification System (0% to 50%, hexane-ethyl acetate) to give 8 mg (57% yield) of the title compound. Purity 98%.

WORKUP

后处理

  1. additionwere added
  2. extractionextracted with ethyl acetate
  3. washThe combined organic phases were washed with water, brine
  4. dry with materialdried over sodium sulphate
  5. customevaporated under reduced pressure
  6. customThe crude was purified by SP1® Purification System (0% to 50%, hexane-ethyl acetate)