反应详情

Step i) 2.00 g (5.87 mM) of 4-(5-dodecylpyrimidine-2-yl)phenol was dispersed in 20 ml of conc. sulfuric acid. To the dispersion, 0.50 ml of nitric acid (60%, density=1.38) was gradually added dropwise under cooling and stirring at 2°-8° C. After the addition, the mixture was stirred for 30 min. at about 5° C. After the reaction, the reaction mixture was poured into 150 ml of iced water to precipitate a crystal. The crystal was recovered by filtration, washed with water and recrystallized from ethanol to obtain 1.85 g of 2-nitro-4-(5-dodecylpyrimidine-2-yl)phenol (yield:81.7%).

1. temperatureunder cooling
2. additionAfter the addition
3. stirringthe mixture was stirred for 30 min. at about 5° C
4. customAfter the reaction
5. customto precipitate a crystal
6. filtrationThe crystal was recovered by filtration
7. washwashed with water
8. customrecrystallized from ethanol