反应详情

To a solution of 2-chloro-4-methyl-6-[4-(trifluoromethyl)phenyl]pyrimidine (which may be prepared as described in Description 11) (167.5 g, 614.34 mmol) in DCM (1325 mL) was added HI (57% in water) (405.23 mL, 3071.7 mmol) dropwise. The reaction was then stirred at room temperature overnight. Additional DCM (500 mL) was added, and the reaction was filtered. The solid was dried then transferred into a beaker containing water (1 L) and EtOAc (1.25 L). The aqueous was basified to pH 10 with K2CO3, and the layers were stirred until all the solid dissolved. Sodium metabisulfite (8.75 g) was added and the layers were stirred until all solid dissolved. The layers were separated, and the aqueous was re-extracted with EtOAc (200 mL). The combined organics were then dried over MgSO4, filtered and concentrated in vacuo to give the title material (D12) (205.68 g, 564.9 mmol, 92% yield) as a pale orange solid. NMR indicated this was >95% pure.

1. filtrationthe reaction was filtered
2. customThe solid was dried
3. additioncontaining water (1 L) and EtOAc (1.25 L)
4. stirringthe layers were stirred until all the solid
5. dissolutiondissolved
6. additionSodium metabisulfite (8.75 g) was added
7. stirringthe layers were stirred until all solid
8. dissolutiondissolved
9. customThe layers were separated
10. extractionthe aqueous was re-extracted with EtOAc (200 mL)
11. dry with materialThe combined organics were then dried over MgSO4
12. filtrationfiltered
13. concentrationconcentrated in vacuo