反应详情

温度

100 °C

32 g (170.04 mmol) of the compound (from example XXVIII) are dissolved in 87.1 ml (0.93 mmol) of phosphoryl chloride. 2.80 ml (22.11 mmol) of N,N-dimethylaniline are slowly added dropwise, and the mixture is stirred at 100° C. for one hour. The reaction solution is then stirred at room temperature for another two hours. The phosphoryl chloride is removed under reduced pressure using a rotary evaporator. Water/dichloromethane 9:1 is added to the residue, which is then boiled for 5 minutes. The mixture is then neutralized using saturated sodium bicarbonate solution and the product is filtered off with suction and dried under high vacuum.

1. stirringThe reaction solution is then stirred at room temperature for another two hours
2. customThe phosphoryl chloride is removed under reduced pressure
3. customa rotary evaporator
4. additionWater/dichloromethane 9:1 is added to the residue, which
5. waitis then boiled for 5 minutes
6. filtrationthe product is filtered off with suction
7. customdried under high vacuum