反应详情

In 3 ml of chloroform was dissolved 0.42 g of 3-[6-(2-butynyloxy)pyrimidin-4-yloxy]-2-methyl-2-butanol, to which 0.2 g of pyridine was added and 0.15 ml of thionyl chloride was added dropwise at −13° C., followed by stirring 2 hours. The reaction mixture was then poured into water, which was extracted three times with chloroform. The combined organic layers were washed with a saturated aqueous sodium hydrogencarbonate, a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.23 g of 4-(2-butynyloxy)-6-(1,2-dimethylallyloxy)pyrimidine.

1. extractionwas extracted three times with chloroform
2. washThe combined organic layers were washed with a saturated aqueous sodium hydrogencarbonate
3. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
4. concentrationconcentrated