HRID1683993

反应详情

EQUATION

反应方程式

HRID 1683993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To the ethyl ester from Example 7, Step 1 (2.00 g, 8.10 mmol) dissolved in THF (40.0 mL) was added at -78° C. a 0.5M solution of KHMDS (16.0 mL, 8.10 mmol) in toluene and HMPA (200 μL). After a period of 10 min, 4-bromobenzyl bromide was added to the resulting mixture. The reaction mixture was brought to room temperature, quenched by the addition of 25% aqueous NH4OAc solution, extracted with EtOAc, dried over Na2SO4 and evaporated in vacuo. The title product was purified by flash chromotography (15% to 20% EtOAc in hexane) (1.5 g).

WORKUP

后处理

  1. customwas brought to room temperature
  2. customquenched by the addition of 25% aqueous NH4OAc solution
  3. extractionextracted with EtOAc
  4. dry with materialdried over Na2SO4
  5. customevaporated in vacuo
  6. customThe title product was purified by flash chromotography (15% to 20% EtOAc in hexane) (1.5 g)