Potassium Nitrate → 5-Bromo-8-nitroisoquinoline

温度

20 °C

Into a 500 mL 3-necked round bottom flask was placed a solution of 5-bromoisoquinoline (22.24 g, 106.87 mmol) in H2SO4 (120 mL). This was followed by the addition of a solution of KNO3 (15.1 g, 149.36 mmol) in H2SO4 (100 mL), which was added dropwise with stirring, while cooling to a temperature of 20° C. over a time period of 1 hour. The resulting solution was allowed to react, with stirring, for 1 hour while the temperature was maintained at room temperature. The reaction progress was monitored by TLC (ethyl acetate/petroleum ether=1:5). The reaction mixture was then quenched by the adding 600 mL of H2O/ice. Adjustment of the pH to 8-10 was accomplished by the addition of NH3. H2O (30%). A filtration was performed. The filter cake was washed 2 times with 500 mL of H2O. The solid was dried in an oven under reduced pressure. This resulted in 25.59 g (90%) of 5-bromo-8-nitroisoquinoline as a yellow solid.

1. customInto a 500 mL 3-necked round bottom flask was placed
2. additionwas added dropwise
3. customto react
4. stirringwith stirring, for 1 hour while the temperature
5. temperaturewas maintained at room temperature
6. customThe reaction mixture was then quenched by the adding 600 mL of H2O/ice
7. additionAdjustment of the pH to 8-10 was accomplished by the addition of NH3
8. filtrationA filtration
9. washThe filter cake was washed 2 times with 500 mL of H2O
10. customThe solid was dried in an oven under reduced pressure
11. customThis resulted in 25.59 g (90%) of 5-bromo-8-nitroisoquinoline as a yellow solid

ORDレコード

ord-7db5e9af87b84bd0b93bea6e49f41bd0

出典データセット

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07696229B2