反应详情

347 g of N-(4,6-dimethoxypyrimidin-5-yl)-chloroacetamide, 60 g benzyltriethylammoniumchloride, 3 l CH2Cl2 and 252 g 1-pyrazolylmethylchloride are charged in a sulphonation flask and thereto added, quickly, 750 ml 30% aqueous NaOH (w/w) while cooling on a ice bath. The reaction temperature rises from 13° to 25°. The reaction mixture is further stirred under continued cooling on the ice bath until the temperature reaches 23°. Then the ice bath is removed and the reaction is stirred further for 2 hours. The reaction mixture is then diluted with 1.5 l of water and stirred. The organic phase is partitioned off, dried with Na2SO4 and filtered over a 6 cm SiO2 layer. The SiO2 -layer is washed with 10 l diethylether. The resulting reaction mixture is concentrated to 1.5 l and the precipitate, which has been falling out is filtered off and washed with pentane, then it is dried under vacuum at 50° to give the title compound m.p. 117°-119°.

1. additionadded
2. customrises from 13° to 25°
3. customreaches 23°
4. customThen the ice bath is removed
5. stirringthe reaction is stirred further for 2 hours
6. additionThe reaction mixture is then diluted with 1.5 l of water
7. stirringstirred
8. customThe organic phase is partitioned off
9. dry with materialdried with Na2SO4
10. filtrationfiltered over a 6 cm SiO2 layer
11. washThe SiO2 -layer is washed with 10 l diethylether
12. customThe resulting reaction mixture
13. concentrationis concentrated to 1.5 l
14. filtrationthe precipitate, which has been falling out is filtered off
15. washwashed with pentane
16. customit is dried under vacuum at 50°