反应详情

23.4 g (0.1 mol) of benzyl-(3-pyridyl)-ketone-hydrochloride are taken up in 180 ml of dimethyl sulphoxide and the solution is treated with 20 ml of 48% hydrobromic acid. The reaction mixture is stirred for 18 hours at 80° - 85°C and subsequently poured on a mixture of 800 g of ice and 1000 ml of water. The yellow emulsion is extracted with 2 × 200 ml of ethyl acetate. The two organic phases are combined, washed with water and dried over sodium sulphate. The red solution is concentrated in a rotary evaporator until a residual oil is left which is distilled in a bulb tube at 140° - 150°C/0.1 Torr (m.p. 56° - 57°C).

1. extractionThe yellow emulsion is extracted with 2 × 200 ml of ethyl acetate
2. washwashed with water
3. dry with materialdried over sodium sulphate
4. concentrationThe red solution is concentrated in a rotary evaporator until a residual oil
5. waitis left which
6. distillationis distilled in a bulb tube at 140° - 150°C/0.1 Torr (m.p. 56° - 57°C)