HRID1845697

反应详情

EQUATION

反应方程式

HRID 1845697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 4,5-dibromo-2-furancarboxylate (4.5 g, 15.85 mmol) and BIS(TRIPHENYLPHOSPHINE)PALLADIUM(II) CHLORIDE (0.38 g, 0.541 mmol) in THF (100 mL) at RT was added chloro(methyl)zinc (15 mL, 30 mmol) dropwise. After stirring for 10 h, the reaction was quenched with NH4Cl (sat'd) (50 mL). The mixture was extracted with EtOAc (50 mL×3), and the collected organic layers were dried over MgSO4. Solvent was removed under vacuum and the resulting residue was purified via column chromatography (silica, EtOAc/Hex 10-20%) to give the title compound (2.5 g, 72%) as a white solid: LC-MS (ES) m/z 220 (M+H)+.

WORKUP

后处理

  1. customthe reaction was quenched with NH4Cl (sat'd) (50 mL)
  2. extractionThe mixture was extracted with EtOAc (50 mL×3)
  3. dry with materialthe collected organic layers were dried over MgSO4
  4. customSolvent was removed under vacuum
  5. customthe resulting residue was purified via column chromatography (silica, EtOAc/Hex 10-20%)