참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Iodine chloride | HCID 24640 | — |
| 반응물 | 2,6-Difluoroaniline | HCID 79647 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 2,6-Difluoro-4-iodoaniline | HCID 278943 | 58.6% |
반응 단계
2,6-Difluoroaniline (38 g) was dissolved in acetic acid (120 ml), and then pyridine (25 g) was added thereto, followed by stirring. Then, a mixture of iodine monochloride (50 g) with acetic acid (30 ml) was added dropwise thereto. After stirring at room temperature for 1 hour, the reaction solution was further stirred at 70° to 80° C. for 2 hours. Then, the reaction solution was poured into water, and the precipitated crystals were filtered, followed by washing with water. The resulting crystals were dissolved in chloroform, and then washed with water twice, further with 10% potassium hydroxide aqueous solution twice, and furthermore with water twice, followed by distilling off chloroform. The residue was distilled under reduced pressure (b.p. 120° to 130° C./20 mmHg), and then recrystallized from methanol to give 4-iodo-2,6-difluoroaniline (44 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05356558 |
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| 출처 데이터셋 | uspto-grants-1994_10 |
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| ORD ID | ord-3e6217ca68cc4b35a55f477b8f50dfb6 |
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| 출처 메모 | uspto-grants-1994_10 |
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