反应详情

温度

90 °C

40 g (0.48 mol) of O-methylhydroxylamine hydrochloride is added to a solution of 100 g (0.44 mol) of 4,6-dichloro-2-methylsulfonylpyrimidine in 400 ml of N,N-dimethylformamide. 66 g (0.48 mol) of potassium carbonate is added and the whole is heated at 90° C. for 10 hours. The mixture is allowed to cool, is evaporated down, the residue is taken up in 10% strength aqueous hydrochloric acid and dichloromethane, the phases are separated, dried and concentrated in a rotary evaporator. The 4-chloro-6-methoxyamino-2-methylsulfonylpyrimidine obtained as byproduct may be separated by chromatography on silica gel (developer: cyclohexane/ethyl acetate). There is obtained 39 g (45%) of the title compound as a white crystalline mass of m.p. 135° C.

1. temperatureto cool
2. customis evaporated down
3. customthe phases are separated
4. customdried
5. concentrationconcentrated in a rotary evaporator