反应详情

3.0 g (10.3 mmol) of (3-chloro-2-chloromethylpyridin-4-yl)-(2-chloroethyl)methylamine hydrochloride and 3.0 g (31 mmol) of potassium acetate are heated at 100° C. for 27 h in 50 ml of glacial acetic acid. The glacial acetic acid is then distilled off and the residue is taken up in 60 ml of ethyl acetate/water (1:1). The mixture is adjusted to pH 8 using sodium bicarbonate solution and extracted with 3×30 ml of ethyl acetate. The organic extracts are washed with water, dried over magnesium sulfate and concentrated. The residue is purified by chromatography on silica gel (eluent: toluenelethyl acetate=1:1). The fractions of Rf =0.25 are concentrated (yield: 1.84 g, 64%) and employed directly for the synthesis of the compound of Example C2.

1. distillationThe glacial acetic acid is then distilled off
2. extractionextracted with 3×30 ml of ethyl acetate
3. washThe organic extracts are washed with water
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customThe residue is purified by chromatography on silica gel (eluent: toluenelethyl acetate=1:1)
7. concentrationThe fractions of Rf =0.25 are concentrated (yield: 1.84 g, 64%)
8. customemployed directly for the synthesis of the compound of Example C2