HRID851907

反应详情

EQUATION

反应方程式

HRID 851907 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.72 ml (3.72 mmol) of a 1M solution of LiAlH4 in THF are added dropwise to a suspension of 577 mg (1.49 mmol) of the product obtained in Step D in 20 ml of THF. The reaction mixture is observed passing into solution and stirring is carried out at ambient temperature for 3 hours. The excess of hydride is hydrolysed by the dropwise addition of water until the evolution of gas ceases. The suspension is stirred for 10 minutes, 20 ml of water are added, and extraction is carried out with AcOEt. The organic phases are combined, washed (saturated NaCl), dried (MgSO4) and evaporated, and the residue is chromatographed on a silica column (CH2Cl2/MeOH 95/5) to yield the title product.

WORKUP

后处理

  1. stirringThe suspension is stirred for 10 minutes
  2. extractionextraction
  3. washwashed (saturated NaCl)
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customthe residue is chromatographed on a silica column (CH2Cl2/MeOH 95/5)