関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dimethyl N-cyanodithioiminocarbonate | HCID 66289 | — |
| 反応物 | 2-Nitrobenzenesulfonamide | HCID 138510 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | methyl N-cyano-N'-(2-nitrophenyl)sulfonylcarbamimidothioate | HCID 178503935 | 55% |
反応手順
A mixture of 2.02 g (10.0 mmol) of 2-nitrobenzene-sulfonamide, 1.46 g (10.0 mmol) of dimethyl N-cyanodithioiminocarbonate and 1.38 g (10.0 mmol) of powdered, anhydrous K2CO3 in 16 ml of acetone was heated at reflux for 20 hours. The reaction mixture was filtered and the solid collected was washed several times with acetone. The filtrate was evaporated and the orange oily residue was triturated with ether to afford a solid. The solid was collected by filtration, washed with ether and suspended in 10 ml of 1N HCl. After stirring for 1 hour the solid was collected by filtration, washed with water and dried to yield 1.65 g (55 percent) of the desired product as a cream colored solid, mp 122° C. (decomposition). IR and 1H NMR spectra were consistent with the assigned structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04650892 |
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| 出典データセット | uspto-grants-1987_03 |
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| ORD ID | ord-c45c01b0436c4bb99bc17aef09665493 |
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| 出典メモ | uspto-grants-1987_03 |
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