HRID2307780

反应详情

EQUATION

反应方程式

HRID 2307780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of Example 34E (3.5 g, 14 mmol) in water (50 mL) was heated to reflux, treated dropwise with a solution of CuSO4 (2.8 g, 17.5 mmol) in water (20 mL), refluxed for 2 hours, cooled to room temperature, adjusted to pH 7 with saturated NaHCO3 (aq), and extracted with ethyl acetate (2×25 mL). The combined extracts were concentrated and the residue was purified by flash column chromatography on silica gel with 1:1 hexanes/ethyl acetate to provide the desired product (0.7 g, 24%).

WORKUP

后处理

  1. temperatureto reflux
  2. temperaturerefluxed for 2 hours
  3. extractionextracted with ethyl acetate (2×25 mL)
  4. concentrationThe combined extracts were concentrated
  5. customthe residue was purified by flash column chromatography on silica gel with 1:1 hexanes/ethyl acetate