反应详情

A solution of 1.62 g (0.01 mol) of benzaldehyde guanylhydrazone and 0.84 g (0.005 mol) of 1-bromo-2-butanone (Aldrich, Buchs, Switzerland; tech. 90%, Cat. no. 24,329-9) in 5 ml of ethanol is stirred for one hour in an ice-water bath and for 16 hours at 20° C. The reaction mixture is then concentrated to dryness by evaporation. The residue is taken up in lethyl acetate, washed twice with water and once with dilute sodium chloride solution, and dried over MgSO4. The ethyl acetate solution is concentrated, whereupon the title compound crystallizes out, m.p. 164°-167° C., 1H-NMR (DMSO): δ=8.41 (s, 1H); 8.89 (m, 2H); 7.46 (m, 3H); 7.13 (s, 1H); 5.9 (s, 2H); 2.34 (q, 2H); 1.13 (t, 3H).

1. concentrationThe reaction mixture is then concentrated to dryness by evaporation
2. washwashed twice with water and once with dilute sodium chloride solution
3. dry with materialdried over MgSO4
4. concentrationThe ethyl acetate solution is concentrated, whereupon the title compound
5. customcrystallizes out