HRID734881

反应详情

EQUATION

反应方程式

HRID 734881 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Under an argon atmosphere 49 mg (0.06 mmol) of PdCl2(dppf) and 11 mg (0.06 mmol) of CuI were added to a repeatedly degassed solution of 535 mg (3.30 mmol) of 2-(4-chlorophenyl)-5-iodopyrazine, 950 mg (3.30 mmol) of 2-(4-ethynylphenoxy)ethanol, and 0.59 mL (6.00 mmol) of piperidine in 50 mL of THF and the mixture was stirred for 4 hours at RT. The precipitate was suction filtered and washed with acetonitrile. The mother liquor was concentrated, and the precipitate formed was filtered off and washed with acetonitrile. The precipitates were combined. Yield: 700 mg (67% of theoretical); C20H15ClN2O2 (M=350.798); calc.: molpeak (M+H)+:351/353 (Cl); found: molpeak (M+H)+:351/353 (Cl); Rf value: 0.30 (silica gel, PE/EtOAc 1:1).

WORKUP

后处理

  1. filtrationfiltered
  2. washwashed with acetonitrile
  3. concentrationThe mother liquor was concentrated
  4. customthe precipitate formed
  5. filtrationwas filtered off
  6. washwashed with acetonitrile