反应详情

12.0 g (35.9 mmol) polymer bound triphenylphosphine and 5.03 mL (35.9 mmol) triethylamine are added to 4.77 g (20.0 mmol) hexachloroethane in 40 mL 1,2-dichloroethane. The mixture is stirred for 5 min at rt. 1.00 g (4.0 mmol) N-(2-chloro-4-hydroxy-pyrimidin-5-yl)-isonicotinamide in 20 mL 1,2-dichloroethane are added and the mixture is stirred for 12 h at rt. Subsequently the mixture is concentrated in vacuo, treated with diethyl ether, filtered, and concentrated again. The residue is purified by HPLC (reversed phase; water (+0.1% TFA)/MeOH) to yield the desired product.

1. stirringthe mixture is stirred for 12 h at rt
2. concentrationSubsequently the mixture is concentrated in vacuo
3. additiontreated with diethyl ether
4. filtrationfiltered
5. concentrationconcentrated again
6. customThe residue is purified by HPLC (reversed phase; water (+0.1% TFA)/MeOH)