反应详情

温度

90 °C

A mixture of 4.42 g (12 mmol) of 1-(4-hydroxy-3,5-dimethylphenyl)piperazine dihydrobromide, 2.84 g (13 mmole) of 4-chloro-5,6-dimethyl-2-phenylpyrimidine, 1.66 g (12 mmol) of powdered K2CO3 and 38 ml of absolute DMF was warmed to 90° C., and 277 mg of powdered K2CO3 were added at 90° C. with stirring in each case after 10 minutes, after a further 25 minutes and after a further 60 minutes (in total 6 mmol of K2CO3), and the mixture was stirred for a further 6 hours at 95° C. The DMF was subsequently removed by distillation in vacuo, the residue was taken up in CH2Cl2 /water, the phases were separated after through mixing, and the aqueous phase was extracted a further three times with CH2Cl2. The combined CH2Cl2 extracts were dried, filtered and evaporated in vacuo. The crystalline residue (5.2 g) was boiled with 15 ml of methanol, and the crystals were filtered off under suction after cooling in an ice bath. In this fashion, 3.54 g (=76% yield) of pure 1-(4-hydroxy-3,5-dimethylphenyl)-4-(5,6-dimethyl-2-phenylpyrimidin-4-yl)piperazine, melting point 188°-89° C., were obtained;

1. customThe DMF was subsequently removed by distillation in vacuo
2. customthe phases were separated after
3. additionthrough mixing
4. extractionthe aqueous phase was extracted a further three times with CH2Cl2
5. dry with materialThe combined CH2Cl2 extracts were dried
6. filtrationfiltered
7. customevaporated in vacuo
8. filtrationthe crystals were filtered off under suction
9. temperatureafter cooling in an ice bath