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Potassium Carbonate → 5-[2-(Dimethylamino)ethyl]-1,3,4-thiadiazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dimethylaminopropionitrile | HCID 15615 | — |
| 反応物 | Thiosemicarbazide | HCID 2723789 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 5-[2-(Dimethylamino)ethyl]-1,3,4-thiadiazol-2-amine | HCID 28065408 | 33% |
反応手順
A solution of 2.00 ml (17.7 mmol) of 3-(dimethylamino)propanenitrile and 1.70 g (18.6 mmol) of thiosemicarbazide in trifluoroacetic acid (5 ml) was heated at 80° C. for 6 hr. The reaction solution was cooled to room temperature and was then diluted with water. The diluted solution was rendered weakly basic by the addition of a 10% aqueous potassium carbonate solution. The solution was extracted with chloroform, and the extract was dried over anhydrous sodium sulfate. The filtrate was concentrated, and the residue was washed with diethyl ether-ethyl acetate to give 1.00 g (yield 33%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07879808B2 |
| 出典データセット | uspto-grants-2011_02 |
| ORD ID | ord-f84e073f8f244555808346b823bba7e4 |
| 出典メモ | uspto-grants-2011_02 |