HRID2063728

反应详情

EQUATION

反应方程式

HRID 2063728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Powdered sodium hydroxide (1.73 g, 43.3 mmol) and tetra-n-butylammonium hydrogen sulfate (111 mg) were added to a solution of the product from stage 1 (6.61 g, 21.6 mmol) in anhydrous methylene chloride (100 ml) and the mixture was stirred at room temperature for 1 h. Benzenesulfonyl chloride (4.21 g, 3.07 ml, 23.8 mmol) was added to the suspension, while cooling with ice. The mixture was stirred at room temperature for 16 h and water and methylene chloride (50 ml of each) were then added. The organic phase was separated off and washed with sodium chloride solution (40 ml). The organic phase was dried with sodium sulfate and concentrated i. vac. The residue was purified by flash chromatography with cyclohexane/ethyl acetate (4:2).

WORKUP

后处理

  1. temperaturewhile cooling with ice
  2. stirringThe mixture was stirred at room temperature for 16 h
  3. customThe organic phase was separated off
  4. washwashed with sodium chloride solution (40 ml)
  5. dry with materialThe organic phase was dried with sodium sulfate
  6. concentrationconcentrated i
  7. customThe residue was purified by flash chromatography with cyclohexane/ethyl acetate (4:2)