HRID327366

反应详情

EQUATION

反应方程式

HRID 327366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of n-butyllithium (10.0M in hexane, 3.30 ml) is added dropwise to a stirred cooled (-78° C.) solution of 3A (9.0 g) in dry THF (70 ml) under dry N2. The stirred mixture is maintained under these conditions for 2.5 h and then a cooled solution of tri-isopropylborate (11.28 g) in dry THF (50 ml) is added dropwise at -78° C. The stirred mixture is allowed to warm to room temperature overnight and then stirred for 1 h at room temperature with 10 HCl (50 ml). The product is extracted into ether twice and the combined ethereal extracts are washed with water and dried (MgSO4). The solvent is removed in vacuo to afford an off-white solid.

WORKUP

后处理

  1. temperatureThe stirred mixture is maintained under these conditions for 2.5 h
  2. extractionThe product is extracted into ether twice
  3. washthe combined ethereal extracts are washed with water
  4. dry with materialdried (MgSO4)
  5. customThe solvent is removed in vacuo
  6. customto afford an off-white solid