反应详情

温度

20 °C

5.1 g (30 mmol) of 5-hydroxy-2-nitrobenzyl alcohol were stirred with 2.5 g (18 mmol) of potassium carbonate and 25 ml of N,N-dimethylacetamide at 70°-80° C. for 30 minutes. After cooling to 20° C., 3.9 ml (36 mmol) of 1-butylbromide were added dropwise and the mixture was stirred at 90° C. for 2 hours. After cooling, the reaction mixture was concentrated in vacuo, the residue was treated with water and the pH was brought to 7 with 2N HCl. The oil obtained crystallizes after about 30 minutes; the product was filtered off with suction, washed with water and dried; 6 g, melting point 47°-49° C.

1. temperatureAfter cooling
2. concentrationthe reaction mixture was concentrated in vacuo
3. additionthe residue was treated with water
4. customThe oil obtained
5. customcrystallizes after about 30 minutes
6. filtrationthe product was filtered off with suction
7. washwashed with water
8. customdried