2-methylbutane-2,3-diol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Is prepared in a similar manner as intermediate III.1 from 2,4-difluoro-1-nitro-benzene and 2-methylbutane-2,3-diol.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Is prepared in a similar manner as intermediate III.1 from 2,4-difluoro-1-nitro-benzene and 2-methylbutane-2,3-diol.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5 g of (+)2 methyl butane 2,3-diol, ##STR24## are mixed with 8.6 g of dichlorophenylphosphin at 0° C. under stirring in 250 ml of dry toluene, in an atmosphere. Then 10.2 g of triethylamine are added within a few minutes. After 1 hour of reaction triethylamine hydrochloride is formed; it is separated by filtration and the toluene solvent is vaporized. is formed it is separated by filtration

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In 5 ml of tetrahydrofuran was suspended 0.24 g of sodium hydride (60% in oil), to which 0.4 ml of a solution containing 0.26 g of 2-methylbutan-2,3-diol in tetrahydrofuran was added dropwise at 0° C., followed by stirring for 10 minutes. To this was added dropwise 0.4 ml of a solution containing 0.38 g of 4,6-dichloropyrimidin in tetrahydrofuran, followed by stirring at 0° C. for 4 hours. To this was added dropwise 0.4 ml of a solution containing 0.20 g of 2-butyn-1-ol and further added 0.12 g of sodium hydride (60% in oil), followed by stirring at room temperature for 3.5 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution, which was extracted three times with t-butyl methyl ether. The combined organic layers were washed with 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 0.41 g of 4-(2-butynyloxy)-6-(2-hydroxy-1,2-dimethylpropyloxy)pyrimidine. was added dropwise at 0° C. by stirring at 0° C. for 4 hours by stirring at room temperature for 3.5 hours was extracted three times with t-butyl methyl ether The combined organic layers were washed with a saturated aqueous sodium chloride solution dried over anhydrous magnesium sulfate concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In 8 ml of tetrahydrofuran was suspended 0.41 g of sodium hydride (60% in oil), to which 0.6 ml of a solution containing 0.49 g of 2-methylbutane-2,3-diol was added dropwise at 0° C., followed by stirring for 10 minutes. To this was added dropwise 0.6 ml of tetrahydrofuran containing 0.69 g of 4,6-dichloropyrimidine dissolved therein, followed by stirring at the same temperature for 4.5 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution, which was extracted three times with t-butyl methyl ether. The combined organic layers were washed with 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 0.74 g of 4-chloro-6-(2-hydroxy-1,2-dimethylpropyloxy)pyrimidine. was added dropwise at 0° C. dissolved by stirring at the same temperature for 4.5 hours was extracted three times with t-butyl methyl ether The combined organic layers were washed with a saturated aqueous sodium chloride solution dried over anhydrous magnesium sulfate concentrated