참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-iodo-N-methyl-2-nitroaniline | HCID 65809849 | — |
| 촉매 | Iron | HCID 23925 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 4-Iodo-N1-methylbenzene-1,2-diamine | HCID 66064280 | 89.7% |
반응 단계
A mixture of an iron powder (1.7 g), acetic acid (2.2 ml), ethanol (80 ml), and water (25 ml) was stirred at 70° C. To the reaction mixture was added dropwise a mixture of (4-iodo-2-nitro-phenyl)-methyl-amine (2.0 g) and ethanol (20 ml). After that, the mixturee was stirred at 70° C. for 6 hours. Then, the reaction mixture was filtrated and thoroughly washed with THF. The resulting filtrate was concentrated under reduced pressure. To the resulting residue was poured saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 4-iodo-N1-methyl-benzene-1,2-diamine (1.6 g)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09120823B2 |
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| 출처 데이터셋 | uspto-grants-2015_09 |
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| ORD ID | ord-8e31494b2f79435f87da827da6172e50 |
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| 출처 메모 | uspto-grants-2015_09 |
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