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Hydrochloric Acid → 1-(2-Aminoethyl)-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 | Ethylenediamine | HCID 3301 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 1,3-Dichloro-2-isothiocyanatobenzene | HCID 123239 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2-Aminoethyl)-3-(2,6-dichlorophenyl)thiourea | HCID 3036787 | — |
反応手順
A solution of 2,6-dichlorophenyl isothiocyanate (500 mg) and THF (5 ml) was added dropwise under argon within 20 minutes to a solution of ethylenediamine (3.68 g) and abs. THF (4 ml). After stirring for a further 30 min, the mixture was added to water, acidified with 10% HCl and extracted three times with ethyl acetate. The aqueous phase was made basic using saturated potassium carbonate solution, and extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulfate, the solvent was removed under reduced pressure and the residue was co-evaporated twice with toluene. After drying in high vacuum, the desired product was obtained as a white solid (532 mg).
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-0c9352ce51844b3ab9f9a5a1d8a82163 |
| 出典メモ | uspto-grants-2014_02 |