참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,3-Dichloropropene | HCID 6565 | — |
| 반응물 | 2-((4-Chlorophenyl)methyl)propanedinitrile | HCID 18082 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(4-Chlorobenzyl)-2-(2-chloro-2-propenyl)malononitrile | HCID 22235025 | 27% |
반응 단계
First, 0.50 g of (4-chlorobenzyl)malononitrile was dissolved in 10 ml of N,N-dimethylformamide, to which 0.16 g of sodium hydride (60% in oil) was added under ice cooling. After the evolution of hydrogen gas ceased, while stirring under ice cooling, 0.48 ml of 2,3-dichloropropene was added dropwise, followed by stirring at room temperature for 5 hours. Then, 10% hydrochloric acid was added to the reaction mixture, which was extracted with diethyl ether. The organic layer was successively washed with 10% hydrochloric acid, a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 0.19 g of 2-(4-chlorobenzyl)-2-(2-chloro-2-propenyl)malononitrile (the present compound (1)).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07402691B2 |
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| 출처 데이터셋 | uspto-grants-2008_07 |
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| ORD ID | ord-6a4c1d8406c64858a00c58cb6370db78 |
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| 출처 메모 | uspto-grants-2008_07 |
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