反应详情

The product of step (c) (10.0 g) was suspended in phosphoryl chloride (55 ml). N,N-dimethylaniline (5.5 ml) added slowly and reaction mixture heated at reflux for 2 hours. Allowed to cool, then poured on to ice with vigorous stirring; temperature was not allowed to go above 45° C. (ice added). After approximately 20 minutes the temperature stabilized at 30° C. The solid that formed was collected by filtration and washed with water. Purified by column chromatography (EtOAc to 5% MeOH in EtOAc) to give 3.34 g of product. 31% yield.

1. customreaction mixture
2. temperatureheated
3. temperatureat reflux for 2 hours
4. temperatureAllowed to cool
5. additionpoured on to ice with vigorous stirring
6. customto go above 45° C.
7. addition(ice added)
8. customThe solid that formed
9. filtrationwas collected by filtration
10. washwashed with water
11. customPurified by column chromatography (EtOAc to 5% MeOH in EtOAc)