HRID473517

反应详情

EQUATION

反应方程式

HRID 473517 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-Bromo-3-fluoro-benzene (1.0 mL, 7.8 mmol), 2-pent-4-ynyl-isoindole-1,3-dione (1.8 g, 8.6 mmol), Pd(PPh3)2Cl2 (191 mg, 0.27 mmol), CuI (118 mg, 0.62 mmol), and triethylamine (4.4 mL, 31.3 mmol) were taken up into DMF (10 mL) and stirred at room temperature for four hours. The reaction was then quenched with saturated NaHCO3 and the resulting mixture extracted with EtOAc and washed with brine, then dried over sodium sulfate and the solvent removed in vacuo. The resulting residue was purified on normal phase chromatography (Heptane/EtOAc) to yield 2-(5-(3-bromophenyl)pent-4-ynyl)isoindoline-1,3-dione. MH+ 368, 370

WORKUP

后处理

  1. customThe reaction was then quenched with saturated NaHCO3
  2. extractionthe resulting mixture extracted with EtOAc
  3. washwashed with brine
  4. dry with materialdried over sodium sulfate
  5. customthe solvent removed in vacuo
  6. customThe resulting residue was purified on normal phase chromatography (Heptane/EtOAc)