反应详情

A mixture of 5-methyl-2,4-bis(4bromophenyl)pyrimidine (8.08 g, 0.02 mole) and copper(I) cyanide (4.45 g, 0.05 mole) in 35 mL dry DMF is refluxed under nitrogen for 40 hr (TLC monitored), the excess DMF is distilled under vacuum using a water aspirator. The residual mass is diluted with water and poured into 200 mL 10% NaCN solution, stirred for 2-3 hr, filtered, washed thoroughly with water, dried and subjected to soxlet extraction using acetone. The acetone is distilled and the residue dissolved into 75 mL CHCl3 and chromatographed over an aluminumoxide column, eluted with ether to 80:20 CHCl3 :ether to yield a white crystalline solid (2.8 g, 48%), mp 194°-195° C.

1. temperatureis refluxed under nitrogen for 40 hr (TLC monitored)
2. distillationthe excess DMF is distilled under vacuum
3. additionThe residual mass is diluted with water
4. additionpoured into 200 mL 10% NaCN solution
5. filtrationfiltered
6. washwashed thoroughly with water
7. customdried
8. extractionextraction
9. distillationThe acetone is distilled
10. dissolutionthe residue dissolved into 75 mL CHCl3
11. customchromatographed over an aluminumoxide column
12. washeluted with ether to 80:20 CHCl3