反应详情

2.07 g sodium hydride (55%) was added in portions to 8.55 g (47.4 mmol) (2R,3R)-3-benzyloxy-butan-2-ol in 56 ml diethyl ether at 0° C. with stirring. After 10 minutes the ice bath was removed and it was stirred for a further 3 minutes at room temperature. The suspension formed was added at 0° C. to a solution of 6.52 g (23.7 mmol) of 2,4-dichloro-5-iodo-pyrimidine. The mixture was stirred for 4 hours at 40° C. and then dilute sodium chloride solution was added. It was then extracted with ethyl acetate (2×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. The residue obtained was chromatographically (hexane/ethyl acetate 4:1). 4.12 g (9.8 mmol; yield: 41%) of the product was obtained.

1. customAfter 10 minutes the ice bath was removed
2. stirringit was stirred for a further 3 minutes at room temperature
3. customThe suspension formed
4. stirringThe mixture was stirred for 4 hours at 40° C.
5. extractionIt was then extracted with ethyl acetate (2×)
6. dry with materialThe combined organic phases were dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated by evaporation
9. customThe residue obtained
10. custom4.12 g (9.8 mmol; yield: 41%) of the product was obtained