反应详情

A solution, cooled to 0° C., of 1 g (3.1 mmol) of the compound from example 17A in 80 ml of CH2Cl2 was admixed dropwise with 1.2 g (6.1 mmol) of bromoacetyl bromide and a little at a time with 1.2 g (9.1 mmol) of AlCl3. The reaction mixture was warmed to room temperature (30 min.) and then heated at reflux for 2 h and carefully poured into ice-water. Following extraction with CH2Cl2, drying over MgSO4 and concentration under reduced pressure, the residue was triturated with ether. This gave 1.33 g (33% pure according to LC-MS) of the desired product which was reacted further without further purification.

1. temperatureheated
2. temperatureat reflux for 2 h
3. extractionextraction with CH2Cl2
4. dry with materialdrying over MgSO4 and concentration under reduced pressure
5. customthe residue was triturated with ether
6. customThis gave 1.33 g (33% pure according to LC-MS) of the desired product which was reacted further without further purification