反应详情

温度

-78 °C

At −78° C., a solution of 34 μl (0.258 mmol) of diethylaminosulphur trifluoride (DAST) in 0.5 ml of anhydrous dichloromethane was added dropwise to a solution of 100 mg (0.215 mmol) of the compound of Example 141 in 4.5 ml of anhydrous dichloromethane. The reaction mixture was stirred at −78° C. for 1 h, about 5 ml of saturated aqueous sodium bicarbonate solution were then added and the mixture was warmed to RT. The mixture was diluted with about 10 ml of water and extracted three times with in each case about 10 ml of dichloromethane. The combined organic extracts were washed once with saturated aqueous sodium chloride solution and dried over magnesium sulphate. After filtration and evaporation, the residue obtained was separated into its components by preparative HPLC (Method 9). Evaporation of the product fractions and drying of the residue under high vacuum gave 40 mg (39% of theory) of the title compound.

1. temperaturethe mixture was warmed to RT
2. extractionextracted three times with in each case about 10 ml of dichloromethane
3. washThe combined organic extracts were washed once with saturated aqueous sodium chloride solution
4. dry with materialdried over magnesium sulphate
5. filtrationAfter filtration and evaporation
6. customthe residue obtained
7. customwas separated into its components by preparative HPLC (Method 9)
8. customEvaporation of the product fractions
9. customdrying of the residue under high vacuum