참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Nitrate | HCID 24434 | — |
| 반응물 | 5-Bromoisoquinoline | HCID 736487 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 5-Bromo-8-nitroisoquinoline | HCID 816983 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07696229B2 |
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| 출처 데이터셋 | uspto-grants-2010_04 |
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| ORD ID | ord-7db5e9af87b84bd0b93bea6e49f41bd0 |
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| 출처 메모 | uspto-grants-2010_04 |
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