関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Dipropylamine | HCID 8902 | — |
| 反応物 | 2,4-Dichloro-1,3-dinitro-5-(trifluoromethyl)benzene | HCID 94398 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Benzenamine, 3-chloro-2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)- | HCID 94399 | 79.6% |
反応手順
A heavy walled glass reaction tube of approximately 50 ml. capacity was charged with 7.0 grams (0.023 mole) of 2,4-dichloro-3,5-dinitrobenzotrifluoride, 4.64 grams (0.0458 mole) of di-n-propylamine and 40 ml. of absolute ethanol. The tube was sealed and heated in an oil bath at 94°-99° C. for 98 hours. The cooled reaction mixture was then evaporated to dryness to give an oily residue which was extracted with boiling diethyl ether. The insoluble di-n-propylamine hydrochloride was removed by filtration and washed with additional ether. The combined ether filtrates were evaporated to give an oily orange residue which was dissolved in 100 ml. of absolute ethanol and decolorized with activated charcoal. The ethanol and volatiles were removed by evaporation under reduced pressure to give the product (6.77 grams) as a viscous reddish oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04046758 |
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| 出典データセット | uspto-grants-1977_09 |
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| ORD ID | ord-e2e92f9dec9049d49fd3125c81de9de5 |
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| 出典メモ | uspto-grants-1977_09 |
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