関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dipropylamine | HCID 8902 | — |
| 反応物 | Ethyl isothiocyanatoformate | HCID 85320 | — |
| 反応物 | 2-N-cyclohexylpyridine-2,3-diamine | HCID 10987083 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl {[2-(cyclohexylamino)-3-pyridyl]imino}(diethylamino)methylcarbamate | HCID 136335149 | — |
反応手順
A mixture of 0.02 mol (3.82 g) of 3-amino-2-cyclohexylaminopyridine from Preparation 1 and 0.02 mol of ethoxycarbonyl isothiocyanate is stirred in 50 ml of DMF at ambient temperature for 3 hours. The solution is then cooled to 0° C., and 0.05 mol of dipropylamine and then 0.02 mol of mercuric chloride are added in succession. After 15 minutes, the ice bath is removed and the solution is stirred at ambient temperature for 4 hours. After diluting the solution with 100 ml of ethyl acetate, filtration is carried out over Celite and the solvents are evaporated off under reduced pressure. The resulting crude product is then recrystallised from acetonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098220B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-b54805a8be0d4495a08ee3d78f19e951 |
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| 出典メモ | uspto-grants-2006_08 |
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