HRID85331

反应详情

EQUATION

反应方程式

HRID 85331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a stream of argon, to 20 ml of tetrahydrofuran was added 1.7 g of phenyllithium (19% solution in dibutylether) (3.83 mmol), and 1.38 g (3.49 mmol) of 2-thenyl triphenylphosphonium chloride was added thereto under ice cooling over 5 minutes. After the mixture was stirred for 10 minutes, 2.07 g (3.49 mmol) of 2-benzyloxy-4-[butyl[4-(tert-butyldiphenylsiloxy)butyl]amino]benzaldehyde dissolved in 50 ml of tetrahydrofuran was added dropwise thereto over 8 minutes. The mixture was stirred under ice cooling for 2 hours. After the reaction mixture was poured into water, extraction with ethyl acetate, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residue was purified by silica gel column chromatography to give 2.03 g of a light brown oily matter (yield: 86.4%).

WORKUP

后处理

  1. additionwas added
  2. additionwas added dropwise
  3. waitover 8 minutes
  4. stirringThe mixture was stirred under ice cooling for 2 hours
  5. washwashing with a saturated saline solution
  6. dry with materialdrying over anhydrous sodium sulfate, and concentration
  7. customThe residue was purified by silica gel column chromatography
  8. customto give 2.03 g of a light brown oily matter (yield: 86.4%)