HRID2059882

反应详情

EQUATION

反应方程式

HRID 2059882 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

tetra-n-Butylammonium chloride (0.33 eq) and sodium hydroxide solution (5 ml/mmol, 35%) were added to a cooled solution of (1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)methanol (1 eq) in toluene (5 ml/mmol) at 0° C. tert-Butylbromoacetate (1.5 eq) was then slowly added dropwise at 0° C. After stirring the mixture at room temperature for 90 min the phases were separated, the organic phase was washed with water to a neutral pH, dried over sodium sulfate and concentrated to small volume under vacuum. The crude product was used in the next stage with no further purification. Yield: 64%

WORKUP

后处理

  1. additionwas then slowly added dropwise at 0° C
  2. customwere separated
  3. washthe organic phase was washed with water to a neutral pH
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to small volume under vacuum
  6. customThe crude product was used in the next stage with no further purification