反应详情

温度

90 °C

To a solution of 9.50 g (72.8 mmol) of 2-chloro-5-hydroxypyrimidine in 100 ml of N,N-dimethylformamide, 26.1 g (80.1 mmol) of cesium carbonate and 24.3 g (102 mmol) of 5-(methanesulfonyloxymethyl)-2,2,5-trimethyl-1,3-dioxane, which was synthesized by the method described in V. W. Gash, Journal of Organic Chemistry, 1972, Vol. 37, pp. 2197-2201, were added, and the reaction solution was stirred at 90° C. for 24 hours. After completion of the reaction, the insoluble material was filtered off and washed with ethyl acetate, and then 0.5 N sodium hydroxide aqueous solution was added to the filtrate and separation was performed. The obtained aqueous layer was further extracted with ethyl acetate. The obtained organic layers were combined, washed with water and saturated sodium chloride aqueous solution in order and dried with anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. Toluene was added to the obtained residue, and the precipitate was obtained by filtration and washed with toluene and n-heptane to provide 6.00 g of the title compound as a white solid (yield: 30%).

1. addition2197-2201, were added
2. customAfter completion of the reaction
3. filtrationthe insoluble material was filtered off
4. washwashed with ethyl acetate
5. addition0.5 N sodium hydroxide aqueous solution was added to the filtrate and separation
6. extractionThe obtained aqueous layer was further extracted with ethyl acetate
7. washwashed with water and saturated sodium chloride aqueous solution in order
8. dry with materialdried with anhydrous magnesium sulfate
9. distillationthe solvent was distilled off under reduced pressure
10. additionToluene was added to the obtained residue
11. customthe precipitate was obtained by filtration
12. washwashed with toluene and n-heptane