反应详情

温度

5 °C

An intimately ground mixture of 5-bromo-2hydroxybenzyl alcohol (4.06 g), 4-nitrobenzaldehyde (3.93 g) and benzoic acid (0.2 g) was stirred and heated to 85° C. (±5° C.) under nitrogen for 88 hours. The clear melt which formed initially gradually solidified throughout the reaction period. The resulting solidified mass was cooled and dissolved in ethyl acetate (250 ml). The solution was then washed with 20% aqueous sodium carbonate, 20% aqueous sodium bisulphite and finally with brine. After drying over sodium sulphate, the organic phase was evaporated to yield a solid residue which was purified by briefly suspending in hot ethanol (approx. 75 ml) and cooling to 0°-5° C. The pure product was obtained as pale buff-coloured crystals (4.69g, 70%), mp 163°-164° C.

1. customThe clear melt which formed initially gradually
2. customsolidified throughout the reaction period
3. temperatureThe resulting solidified mass was cooled
4. washThe solution was then washed with 20% aqueous sodium carbonate, 20% aqueous sodium bisulphite and finally with brine
5. dry with materialAfter drying over sodium sulphate
6. customthe organic phase was evaporated
7. customto yield a solid residue which
8. customwas purified
9. temperaturecooling to 0°-5° C