反应详情

A mixture of the product from Step 2 (4.7 g, 18.5 mmol) in phosphorus oxychloride (30 mL) was heated to reflux for 2 hours and cooled to RT; the volatiles were evaporated; and the residue was partitioned between 3 M NaOH and DCM. The organic phase was dried over Na2SO4; the solvent was evaporated; and the solid was triturated with Et2O (20 mL) and filtered to give the title compound (3.75 g). LRMS ESI+ (M+H)+ 274.0.

1. temperaturewas heated
2. temperatureto reflux for 2 hours
3. customthe volatiles were evaporated
4. customand the residue was partitioned between 3 M NaOH and DCM
5. dry with materialThe organic phase was dried over Na2SO4
6. customthe solvent was evaporated
7. customand the solid was triturated with Et2O (20 mL)
8. filtrationfiltered