反应详情

温度

-10 °C

A solution of 24.85 g (117.5 mmol) of 2,4-dichloro-pyrimidine-5-carbonyl chloride in 125 ml of THF is cooled to −15° C. It is slowly mixed with a solution of 13.2 ml (124.5 mmol) of tert-buylamine and 17.4 ml (125.7 mmol) of triethylamine in 50 ml of THF, so that the temperature of the reaction mixture remains less than −10° C. It is stirred for another 2 hours at −10° C., then the cooling bath is removed, and the reaction mixture is heated to room temperature while being stirred. After 1 hour, the precipitate that is formed is filtered off, and the filtrate is completely concentrated by evaporation. The residue that is obtained is purified by chromatography (hexane/ethyl acetate 4:1). 14.01 g (56.6 mmol, corresponding to 50% of theory) of the product is obtained.

1. customremains less than −10° C
2. customthe cooling bath is removed
3. temperaturethe reaction mixture is heated to room temperature
4. stirringwhile being stirred
5. waitAfter 1 hour
6. customthe precipitate that is formed
7. filtrationis filtered off
8. concentrationthe filtrate is completely concentrated by evaporation
9. customThe residue that is obtained
10. customis purified by chromatography (hexane/ethyl acetate 4:1)
11. custom14.01 g (56.6 mmol, corresponding to 50% of theory) of the product is obtained