HRID1106935

反应详情

EQUATION

反应方程式

HRID 1106935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyldimethylchlorosilane (5.10 g, 33.8 mmol) was added to a solution of 2-nitrocinnamyl alcohol (5.05 g, 28.2 mmol) and imidazole (2.88 g, 42.3 mmol) in DMF (100 ml). After stirring at room temperature for 18 hours the reaction mixture was partitioned between water (200 ml) and ethyl acetate (200 ml). The organic layer was separated washed with brine (2×m 100 ml) and dried (MgSO4). Filtration and evaporation of the solvent gave the crude product which was purified by flash chromatography on silica gel with ethyl acetate-hexane (1:3) as eluant. (7.82 g, 95%).

WORKUP

后处理

  1. customwas partitioned between water (200 ml) and ethyl acetate (200 ml)
  2. customThe organic layer was separated
  3. washwashed with brine (2×m 100 ml)
  4. dry with materialdried (MgSO4)
  5. filtrationFiltration and evaporation of the solvent