反应详情

To a mixture of 98 grams of 2-(1,1-dimethylethyl)-5-pyrimidinol, 130 grams of finely powdered potassium carbonate and 800 ml of acetonitrile was added 121 grams of O,O-diethyl phosphorochloridothioate. The temperature of the reaction mixture rose to 55° C. Stirring was continued until no more starting O,O-diethyl phosphorochloridothioate could be detected by gas-liquid chromatography. The reaction appeared to be complete in about 1 hour. The salts present were then removed by filtration, the filtrate concentrated in a rotary evaporator, the residue taken up in ether, the ether solution washed twice with 2 percent aqueous sodium hydroxide, and once with saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The ether was then removed under vacuum leaving a pale yellow colored oil with a refractive index at 25° of 1.4913. On elemental analysis the product was found to contain by weight 47.38% carbon; 6.67% hydrogen and 9.19% nitrogen. Theoretical analysis is 47.35% carbon; 6.96% hydrogen and 9.21% nitrogen.

1. customrose to 55° C
2. customThe salts present were then removed by filtration
3. concentrationthe filtrate concentrated in a rotary evaporator
4. washthe ether solution washed twice with 2 percent aqueous sodium hydroxide
5. dry with materialonce with saturated sodium chloride solution, and dried over anhydrous sodium sulfate
6. customThe ether was then removed under vacuum
7. customleaving a pale yellow colored oil with a refractive index at 25° of 1.4913