HRID1004073

反应详情

EQUATION

反应方程式

HRID 1004073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of (R)-(3-chloro-phenyl)-(tert-butyl-dimethyl-silanoxy)-acetic acid methyl ester (4.0 g) in anhydrous ether (10 ml) and maintained at <-65° was added dropwise a 1.5M solution of di-isobututylaluminium hydride in toluene (10 ml). When addition was complete the solution was stirred at -65° for a further hour, then quenched with methanol (10 ml). The mixture was allowed to attain room temperature when silica (20 g) was added. Solvent was removed under reduced pressure, and the residue was purified by flash chromatography, eluting with cyclohexane:ethyl acetate (9:1) to give the title compound as a colourless liquid (3.1 g).

WORKUP

后处理

  1. additionWhen addition
  2. customquenched with methanol (10 ml)
  3. customto attain room temperature
  4. additionwas added
  5. customSolvent was removed under reduced pressure
  6. customthe residue was purified by flash chromatography
  7. washeluting with cyclohexane:ethyl acetate (9:1)