反应详情

To a solution of 4,6-dichloro-2-[(2,3-difluorobenzyl)thio]pyrimidine ((the product of example 1 step ii), 5 g) and ethylene glycol (1.517 g) in THF (100 ml) was added NaH (1.3 g) slowly and the reaction was then allowed to stir overnight at RT. The reaction mixture was then partitioned between EtOAc (200 ml) and H2O (200 ml). The organics were separated and the aqueous layer was re-extracted with EtOAc (2×200 ml). Organics were combined, dried (MgSO4) and reduced in vacuo and the resulting residue was purified by column chromatography on silica gel 10% EtOAc/90% iso-Hex to give the subtitle compound as a clear oil. Yield: 2.4 g

1. customThe reaction mixture was then partitioned between EtOAc (200 ml) and H2O (200 ml)
2. customThe organics were separated
3. extractionthe aqueous layer was re-extracted with EtOAc (2×200 ml)
4. dry with materialdried (MgSO4)
5. customthe resulting residue was purified by column chromatography on silica gel 10% EtOAc/90% iso-Hex