HRID1052522

反应详情

EQUATION

反应方程式

HRID 1052522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

4-Chloro-5-iodo-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidine (50 mg, 0.12 mmol) was dissolved in 140 μl tetrahydrofuran and 160 μl triethylamine. Ethynylbenzene (16 μl, 0.15 mmol), bis(triphenylphosphine)palladium(II) dichloride (9 mg, 0.01 mmol) and copper(I) iodide (5 mg, 0.02 mmol) were added and the mixture was stirred at room temperature during 2 h. The reaction was poured into a 4% aqueous solution of sodium bicarbonate and extracted twice with ethyl acetate. The organics were combined and washed with water, brine, dried over sodium sulphate, filtered and evaporated under reduced pressure. The residue was purified using SP1® Purification System (0% to 15%, hexane-ethyl acetate) to give 45 mg (95% yield) of the title compound.

WORKUP

后处理

  1. extractionextracted twice with ethyl acetate
  2. washwashed with water, brine
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified
  7. customSP1® Purification System (0% to 15%, hexane-ethyl acetate)