HRID623665

反应详情

EQUATION

反应方程式

HRID 623665 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,5-bis-benzyloxy-2-isopropyl-4-azido-benzene (890 mg, 2.38 mmol) was dissolved in DMF (5 ml) and (4-ethynylphenyl)-methanol (286 mg, 2.16 mmol) was added at RT. The flask was subjected to three vacuum-nitrogen cycles. [Cp*RuCl]4 was then added (116 mg, 0.11 mmol) and three further cycles were done. The reaction was left to RT until completion (monitored by TLC). AcOEt and water were then added. The organic phase was extracted four times with AcOEt, washed with water (three times) and brine (one time) and dried over Na2SO4; the solvent was removed under reduced pressure and the mixture was purified by column chromatography (PE/AcOEt: 60:40). The title compound was obtained as an oil.

WORKUP

后处理

  1. waitThe reaction was left to RT until completion (monitored by TLC)
  2. extractionThe organic phase was extracted four times with AcOEt
  3. washwashed with water (three times) and brine (one time)
  4. dry with materialdried over Na2SO4
  5. customthe solvent was removed under reduced pressure
  6. customthe mixture was purified by column chromatography (PE/AcOEt: 60:40)