関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 1,2-Ethanediamine, 4-methylbenzenesulfonate (1:?) | HCID 225030 | — |
| 反応物 | 4-(Cyanomethoxy)benzonitrile | HCID 20529061 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 生成物 | HCID 20529046 | HCID 20529046 | — |
反応手順
A mixture of 15.8 g of 4-cyanophenoxyacetonitrile and 23.3 g of ethylenediamine p-toluenesulfonate in 50 ml of 1,2-dichlorobenzene was heated at from about 130°-145° C. for about an hour. After reaction the mixture was cooled, diluted with CH2Cl2 and filtered to obtain the crude product. The crude product was dissolved in boiling absolute ethanol, treated with activated charcoal and filtered through a fluted paper. The filtrate was cooled to 5° C. for 1.5 hours and the crystals which formed removed by filtering. After drying in a vacuum oven, off-white crystals were obtained having a melting point of 190°-192° C. The off-white crystals were put in solution in 200 ml of boiling water and treated with activated charcoal and filtered. The filtrate was cooled to 5° C. for 1 hour and the crystals which formed removed by filtration. Upon drying, the product 2-((4-cyanophenoxy)methyl)-2-imidazoline p-toluenesulfonate was obtained as white crystals, m.p. 196°-198° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04343808 |
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| 出典データセット | uspto-grants-1982_08 |
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| ORD ID | ord-eb7a0cf14e554f1c8b942e4242ebdfe8 |
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| 出典メモ | uspto-grants-1982_08 |
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