HRID656888

反应详情

EQUATION

反应方程式

HRID 656888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of 7-quinolinyl trifluoromethanesulfonate (1.88 g, 6.8 mmol) in DMF (40 ml) was degassed for 10 minutes with Argon. Zinc(II) cyanide (0.48 g, 4.08 mmol), tris(dibenzylideneacetone)dipalladium(0) (155 mg, 2.5% mmol) and 1,1′-bis(diphenylphospino)ferrocene (188 mg, 5% mmol) was then added and the mixture was heated at 100° C. under argon for 1.5 h. The solvent was evaporated and residue dissolved in DCM and organic phase washed with a saturated solution of sodium bicarbonate. The aqueous phase was extracted with DCM (3×80 ml). The combined organic phases were dried, evaporated and the residue was chromatographed on silica gel, eluting with 0-10% methanol-DCM to afford the desired compound (1.01 g, 97%).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionresidue dissolved in DCM
  3. washorganic phase washed with a saturated solution of sodium bicarbonate
  4. extractionThe aqueous phase was extracted with DCM (3×80 ml)
  5. customThe combined organic phases were dried
  6. customevaporated
  7. customthe residue was chromatographed on silica gel
  8. washeluting with 0-10% methanol-DCM