참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Sodium amide | HCID 24533 | — |
| 반응물 | 3-Methyl-2-butenenitrile | HCID 94301 | — |
| 반응물 | 4-Diisopropylamino 2-(2-pyridyl)butyronitrile | HCID 13319674 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 2-(2-Diisopropylamino ethyl) 3,3-dimethyl 2-(2-pyridyl) pentane-dinitrile | HCID 54234562 | — |
반응 단계
The mixture of 4.7 g of sodium amide and 400 ml of liquid ammonia is cooled to -40° C., then the solution of 24.5 g of 4-diisopropylamino 2-(2-pyridyl) butane nitrile (Example 1a) in 30 ml of anhydrous ether is added, the temperature being maintained between -40° C. and -33° C. The mixture is stirred for 15 mins. at this temperature then the solution of 9 g of 3,3-dimethyl acrylonitrile in 40 ml of ether is added, still at the same temperature. The temperature is allowed to rise slowly up to ambient temperature (duration: about 5 hrs.). 200 ml of ether are added then water is added drop by drop. The ethereal phase is separated and the aqueous phase is re-extracted with ether. The ethereal extracts are collected and dried over sodium sulfate. The solvent is evaporated to dryness and the residue is chromatographed over a column of alumina with the eluting ethyl acetate-pentane (2.5-100) vol/vol mixture.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04721710 |
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| 출처 데이터셋 | uspto-grants-1988_01 |
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| ORD ID | ord-b58ef02f0aaf4f5d8b614354929b82db |
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| 출처 메모 | uspto-grants-1988_01 |
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