참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Hexadecylamine | HCID 8926 | — |
| 반응물 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | chloroform N,N-dimethylformamide | HCID 21754633 | — |
| 생성물 | 2-Hexadecylamino-5-nitropyridine | HCID 22155764 | — |
반응 단계
0.5 g (3.2 mmol) of 2-chloro-5-nitropyridine (Fluka, purum), 0.76 g (3.2 mmol) of hexadecylamine (Merck-Schuchard, for synthesis) and 1 g of NaHCO3 are weighed out and suspended in 10 ml of CHCl3 /DMF 1:1 (puriss., for analysis). The suspension is heated to 100° C. (bath temperature) and stirred for 4 hours at this temperature. When the reaction mixture has cooled, water is added and extraction is carried out with diethyl ether. The organic phase is extracted twice with water and dried over Na2SO4. After evaporation of the solvent, the residue is chromatographed on 50 times the amount of silica gel (eluent=hexane/ether 95:5). The slightly yellowish product fraction is concentrated and 1 is recrystallized again from hexane/ether.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04973429 |
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| 출처 데이터셋 | uspto-grants-1990_11 |
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| ORD ID | ord-c314f438f6134fd9930e87a1cbeaee9e |
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| 출처 메모 | uspto-grants-1990_11 |
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