참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | 2-Nitropyridin-3-amine | HCID 83281 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 6-Bromo-2-nitropyridin-3-amine | HCID 56587806 | 64.3% |
반응 단계
To a stirred suspension of 2-nitro-pyridin-3-ylamine (5.06 g, 36.40 mmol) and sodium acetate (2.99 g, 36.46 mmol) in acetic acid (40 mL), a solution of bromine (2.5 mL, 48.79 mmol) in acetic acid (8 ml) was added drop-wise and the reaction mixture was stirred overnight. The acetic acid was removed under reduced pressure. The residue was cooled to 0° C., neutralized with saturated sodium bicarbonate solution to adjust the pH to ˜7, and extracted with ethyl acetate (4×50 mL). The combined organic extracts were washed with brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The residue was triturated with ethyl acetate to afford compound (5) (5.1 g) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09309267B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-3f601925248643048203571bed82ebba |
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| 출처 메모 | uspto-grants-2016_04 |
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