HRID1963063

反应详情

EQUATION

反应方程式

HRID 1963063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of the compound of example 5, step 5 (0.955 g, 1.67 mmol) in 10 ml of DCM under argon was added 1,1,1-triacetoxy-1,1-dihydro-1,2-benziodoxol-3(1H)-one (7.78 g, 1.84 mmol). The mixture was stirred at room temperature for 3.5 h and then diluted with 40 ml of diethyl ether. The solution was washed three times with a 1 N solution of sodium hydroxide (15 ml) and twice with brine (15 ml). The organic phase was dried over sodium sulfate, filtered and evaporated to dryness under reduced pressure to give 0.965 g of the title compound as a green powder which was directly used in the next step.

WORKUP

后处理

  1. washThe solution was washed three times with a 1 N solution of sodium hydroxide (15 ml)
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated to dryness under reduced pressure