참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | 4,6,6,6-Tetrachloro-2-cyano-3,3-dimethylhexanoic acid | HCID 20434843 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-(2,2-Dichloroethenyl)-2,2-dimethylcyclopropane-1-carbonitrile | HCID 12898173 | 89% |
반응 단계
A solution of 4-chloro-2-cyano-3,3-dimethyl-6,6,6-trichlorohexanoic acid (6.14 g) in dimethyl formamide (12 ml) was stirred at 145° C. for 4 hours under an ammonia atmosphere at initially 5 bar pressure. After release of the pressure the mixture was stirred for another 6 hours at 145° C. After cooling, over 90% of the solvent was flashed off (bath temperature max. 60° C., pressure 12 mmHg). The residue was mixed with toluene and subsequently washed with aqueous hydrochloric acid and aqueous sodium bicarbonate. After drying of the organic phase the solvent was removed under reduced pressure to yield 3.3 g of the required 2-(2,2-dichlorovinyl)-3,3-dimethylcyclopropane nitrile (97% pure, 89% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04211720 |
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| 출처 데이터셋 | uspto-grants-1980_07 |
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| ORD ID | ord-53db2e25760d41c08e88f52e34312f8c |
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| 출처 메모 | uspto-grants-1980_07 |
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