(3R)-2-甲基丁烷-2,3-二醇

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.84 g (42.3 mmol) of sodium hydride (55%) was added in portions, with stirring at 0° C., to a solution of 4.40 g (42.3 mmol) (R)-2-methyl-butane-2,3-diol in 83 ml diethyl ether and was stirred for 10 minutes. It was stirred for a further 3 minutes at room temperature and the mixture was then added to an ice-cooled solution of 9.68 g (35.2 mmol) of 2,4-dichloro-5-iodo-pyrimidine in 97 ml acetonitrile. The mixture was stirred for 4 hours at 40° C. and, after cooling, ice and saturated NaCl solution were added. It was then extracted with ethyl acetate (3×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. The residue obtained was purified chromatographically (hexane/ethyl acetate 4:1). 4.96 g (14.5 mmol; yield: 41%) of the product was obtained. It was stirred for a further 3 minutes at room temperature The mixture was stirred for 4 hours at 40° C. after cooling It was then extracted with ethyl acetate (3×) The combined organic phases were dried (Na2SO4) filtered concentrated by evaporation The residue obtained was purified chromatographically (hexane/ethyl acetate 4:1) 4.96 g (14.5 mmol; yield: 41%) of the product was obtained

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.84 g (42.3 mmol) of sodium hydride (55%) was added in portions, with stirring at 0° C., to a solution of 4.40 g (42.3 mmol) (R)-2-methyl-butane-2,3-diol in 83 ml diethyl ether and was stirred for 10 minutes. It was stirred for a further 3 minutes at room temperature and the mixture was then added to an ice-cooled solution of 9.68 g (35.2 mmol) of 2,4-dichloro-5-iodo-pyrimidine in 97 ml acetonitrile. The mixture was stirred for 4 hours at 40° C. and, after cooling, ice and saturated NaCl solution were added. It was then extracted with ethyl acetate (3×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. The residue obtained was purified chromatographically (hexane/ethyl acetate 4:1). 4.96 g (14.5 mmol; yield: 41%) of the product was obtained. It was stirred for a further 3 minutes at room temperature The mixture was stirred for 4 hours at 40° C. after cooling It was then extracted with ethyl acetate (3×) The combined organic phases were dried (Na2SO4) filtered concentrated by evaporation The residue obtained was purified chromatographically (hexane/ethyl acetate 4:1) 4.96 g (14.5 mmol; yield: 41%) of the product was obtained