反应详情

温度

150 °C

60 mg of sodium were added to 2 ml of ethylene glycol at 70° C. Thereafter, 223 mg of N-[6-chloro-5-(2,6-dimethoxybenzyl)-4-pyrimidinyl]-p-vinyl-benzenesulfonamide were added and the reaction mixture was heated at 150° C. for 4.5 hours. The ethylene glycol was distilled under reduced pressure, the residue was taken up in EtOAc/H2O and extracted once with ethyl acetate. Thereafter, the aqueous phase was acidified with 1N HCl and extracted four times with ethyl acetate. The organic phase was dried, filtered and concentrated under reduced pressure. The residue was chromatographed over 50 g of SiO2 with methylene chloride/ethyl acetate 1:1. There were obtained 50 mg of N-[5-(2,6-dimethoxybenzyl)-6-(2-hydroxyethoxy)-4-pyrimidinyl]-p-vinylbenzenesulfonamide, melting point 138°-139° C.

1. distillationThe ethylene glycol was distilled under reduced pressure
2. extractionextracted once with ethyl acetate
3. extractionextracted four times with ethyl acetate
4. customThe organic phase was dried
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was chromatographed over 50 g of SiO2 with methylene chloride/ethyl acetate 1:1