反应详情

温度

0 °C

20.0 g (69.6 mmol) of the compound from Example 2A were dissolved in 1.0 l of dichloromethane and admixed at 0° C. with 14.1 g (139 mmol) of triethylamine. Subsequently, 14.0 g (69.6 mmol) of 4-nitrophenyl chlorocarbonate were added dropwise. The reaction mixture was stirred at 0° C. for 2 h and then at RT for 16 h. For workup, the mixture was washed with saturated aqueous sodium hydrogencarbonate solution. The organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. This gave 31.3 g of crude product, which was reacted without any further purification steps.

1. waitat RT for 16 h
2. washFor workup, the mixture was washed with saturated aqueous sodium hydrogencarbonate solution
3. dry with materialThe organic phase was dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThis gave 31.3 g of crude product, which was reacted without any further purification steps