HRID2250407

反应详情

EQUATION

反应方程式

HRID 2250407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A slurry of the product of step (b) (1.39 g), 8-(benzyloxy)-5-[(R)-2-bromo-1-(tert-butyldimethylsilanyloxy)ethyl]-1H-quinolin-2-one (2.49 g), sodium iodide (1.14 g) and potassium carbonate (2.11 g) in DMSO (7 mL) was heated at 90° C. for 5 h. The solution was allowed to cool, diluted with dichloromethane (60 mL) and washed with water (4×30 mL) then brine (40 mL). The organics were dried over sodium sulfate, concentrated in vacuo and the residue purified by reverse phase HPLC to afford the title intermediate (1.85 g) as a clear oil. m/z: [M+H+] calcd for C38H43ClN2O4Si 655.3. found 655.5.

WORKUP

后处理

  1. temperatureto cool
  2. washwashed with water (4×30 mL)
  3. dry with materialThe organics were dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customthe residue purified by reverse phase HPLC