참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 2,6-Dimethylnitrobenzene | HCID 6672 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-Iodo-2,4-dimethyl-3-nitrobenzene | HCID 2324887 | 236.9% |
반응 단계
To 1,3-dimethyl-2-nitro-benzene (68.5 g, 453.2 mmol) is added sulfuric acid (27.2 mL, 510 mmol), acetic acid (543.8 mL, 9.49 mol), iodine (46 g, 181.3 mmol) and HIO4 (91.9 g, 403.3 mmol). The reaction is heated to 90° C. for 7 days. The reaction mixture is cooled to ambient temperature and water (500 mL) is added. The resulting solid is collected by filtration and washed with cold water. The solid is dried under reduced pressure at 45° C. overnight to afford the title compound as a yellow solid (119 g, 95%). 1H NMR (300.16 MHz, CDCl3): δ 7.80 (d, J=8.2 Hz, 1H), 6.85 (d, J=8.2 Hz, 1H), 2.37 (s, 3H), 2.23 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08642768B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-d0b62ca0fd454239a7d154c07cd94bce |
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| 출처 메모 | uspto-grants-2014_02 |
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