反应详情

温度

-20 °C

5-(3-Ethoxy-5-hydroxy-4-iodo-benzyl)-pyrimidine-2,4-diamine (see example 32 stage a) (2,300 mg; 5.96 mmol) is dissolved in tetrahydrofuran (70 ml), potassium tert-butylate (1,000 mg; 8.9 mmol) is added and the mixture is cooled to −20° C. Tetrahydropyran-4-sulphonyl chloride (2.2 g; 11.9 mmol) is added at this temperature and the mixture is then stirred for one hour at −20° C. The reaction mixture is poured on to ice-water and extracted twice with ethyl acetate. The organic phase is dried over sodium sulphate, the salts are filtered off and the solvent is evaporated off. The residue is chromatographed over silica gel with methylene chloride 1 methanol (19/1) and 0.5% ammonia. The pure fractions are co mbidand the solvent is evaporated off.

1. extractionextracted twice with ethyl acetate
2. dry with materialThe organic phase is dried over sodium sulphate
3. filtrationthe salts are filtered off
4. customthe solvent is evaporated off
5. customThe residue is chromatographed over silica gel with methylene chloride 1 methanol (19/1) and 0.5% ammonia
6. customis evaporated off