反应详情

温度

100 °C

Phosphorous oxychloride (5.45 mL, 58.5 mmol) was added to a slurry of 6-bromo-3-nitroquinolin-4-ol (15 g, 55.7 mmol) in N,N-dimethylformamide (100 mL). The reaction mixture was heated to 100° C. for 10 minutes and then cooled to ambient temperature. The solution was poured into ice water (400 mL) and stirred for 20 minutes. The resulting precipitate was filtered, washed with water, and dried. The recovered solid was transferred to a round bottomed flask and tetrahydrofuran (100 mL) was added. A solution of triethylamine (11.6 mL, 83.5 mmol) and 1-amino-2-methylpropan-2-ol (5.21 g, 58.5 mmol) in tetrahydrofuran (20 mL) was added dropwise. The reaction was stirred for 16 hours. The mixture was poured into water and stirred for 15 minutes. The resulting yellow solid was filtered and dried to provide 17.2 g of 1-[(6-bromo-3-nitroquinolin-4-yl)amino]-2-methylpropan-2-ol as a yellow solid.

1. temperaturecooled to ambient temperature
2. filtrationThe resulting precipitate was filtered
3. washwashed with water
4. customdried
5. customThe recovered solid was transferred to a round bottomed flask
6. additiontetrahydrofuran (100 mL) was added
7. stirringThe reaction was stirred for 16 hours
8. stirringstirred for 15 minutes
9. filtrationThe resulting yellow solid was filtered
10. customdried