참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon Tetrachloride | HCID 5943 | — |
| 반응물 | Chlorine | HCID 24526 | — |
| 반응물 | 2-Bromo-5-methylpyridine | HCID 564216 | — |
| 생성물 | 2-Chloro-5-trichloromethylpyridine | HCID 50293 | — |
반응 단계
172 g of thus obtained 2-bromo-5-methylpyridine was dissolved in 1.3 l of carbon tetrachloride, and the system was then heated. At the time refluxing begain (at 77° C.), chlorine gas was bubbled into the system with ultraviolet light irradiation. After a lapse of 5 hours, the completion of the reaction was confirmed by gas chromatography, and the system was cooled and air was bubbled into the system to expel the unreacted chlorine. The system was washed with water several times and dried over anhydrous sodium sulfate. Then, the carbon tetrachloride was distilled off, and the system was allowed to cool. The solid crystals thus-obtained were washed with n-hexane to obtain 152 g of 2-chloro-5-trichloromethylpyridine with a melting point of 51° to 54° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04184041 |
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| 출처 데이터셋 | uspto-grants-1980_01 |
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| ORD ID | ord-8fa83cdffa03461b884acc299e5cd297 |
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| 출처 메모 | uspto-grants-1980_01 |
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