HRID858520

反应详情

EQUATION

反应方程式

HRID 858520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 4-bromophenethylalcohol (5.00 g, 24.9 mmol) in THF (80 ml) was added a solution of 1.5M n-BuLi in hexane (39.8 ml, 59.7 mmol) at −78° C. over 30 min. After 1 hour, a solution of B(OiPr)3 (8.61 ml, 37.3 mmol) in THF (20 ml) was added slowly to the mixture at −78° C. The resultant mixture was warmed to room temperature, and treated with 2M HCl (100 ml) for 1 hour. This was extracted with CH2Cl2 and dried over MgSO4, then filtered. After evaporation in vacuo, the residue was purified by silica-gel column chromatography eluting with CH2Cl2/MeOH=20/1 to afford 2.61 g (63%) of the title compound.

WORKUP

后处理

  1. extractionThis was extracted with CH2Cl2
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customAfter evaporation in vacuo
  5. customthe residue was purified by silica-gel column chromatography
  6. washeluting with CH2Cl2/MeOH=20/1