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Hydrochloric Acid → 1-(2-Aminocyclohexyl)-3-(2,6-dichlorophenyl)thiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 1,2-Diaminocyclohexane, trans- | HCID 43806 | — |
| 反応物 | 1,3-Dichloro-2-isothiocyanatobenzene | HCID 123239 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2-Aminocyclohexyl)-3-(2,6-dichlorophenyl)thiourea | HCID 86595209 | 82.1% |
反応手順
A solution of 1,3-dichloro-2-isothiocyanatobenzene (100 mg) and abs. THF (3 ml) was added dropwise slowly over a half hour to a solution of trans-1,2-diaminocyclohexane (139.9 mg) and abs. THF (3 ml). The solution was stirred at room temperature for a further 90 minutes. The reaction mixture was subsequently added to water, acidified with hydrochloric acid and extracted once with ethyl acetate. Afterwards, the mixture was basified using potassium carbonate, and extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulfate, filtered and concentrated. 128 mg of the desired product were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653259B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-43534b07de5b47c4bf5d893c09df7a0a |
| 出典メモ | uspto-grants-2014_02 |