HRID1527891

反应详情

EQUATION

反应方程式

HRID 1527891 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A mixture of ethyl 3-iodo-4-methylbenzoate (845 mg, 2.9 mmol, 0.8 eq), N-(5-ethynylpyridin-2-yl)acetamide (3.5 mmol, 1.0 eq), Pd(PPh3)4 (51 mg, 0.044 mmol), CuI (20.4 mg, 0.11 mmol), and N,N-diisopropylethylamine (0.8 ml, 4.4 mmol) in 2 ml of DMF is heated at 55° C. (oil bath) for 1 hr under nitrogen. After cooling to r.t., the solvent is evaporated and DCM is added to dissolve the residue. The solution is washed with water and brine, dried and evaporated and the crude material is chromatographed with CombiFlash (DCM/MeOH).

WORKUP

后处理

  1. temperatureAfter cooling to r.t.
  2. customthe solvent is evaporated
  3. additionDCM is added
  4. dissolutionto dissolve the residue
  5. washThe solution is washed with water and brine
  6. customdried
  7. customevaporated
  8. customthe crude material is chromatographed with CombiFlash (DCM/MeOH)