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Water → 5-(2-((2-(5-Amino-1,3,4-thiadiazol-2-yl)ethyl)amino)ethyl)-1,3,4-thiadiazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3,3'-Iminodipropionitrile | HCID 8149 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Thiosemicarbazide | HCID 2723789 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 5-(2-((2-(5-Amino-1,3,4-thiadiazol-2-yl)ethyl)amino)ethyl)-1,3,4-thiadiazol-2-amine | HCID 3950759 | 44.5% |
反応手順
A mixture of 3,3′-iminodipropionitrile (1.50 g, 12.18 mmol) and thiosemicarbazide (2.22 g, 24.36 mmol) in TFA (10 mL) was heated at 85 for 4.5 h. The reaction was cooled to room temperature and poured into a mixture of ice and water. Sodium hydroxide pellets were added to the mixture until it was basic (pH 14). The white precipitate was collected by suction filtration, rinsed with water and dried to provide 5-(2-((2-(5-amino-1,3,4-thiadiazol-2-yl)ethyl)amino)ethyl)-1,3,4-thiadiazol-2-amine (1005, 1.47 g). 1H NMR (300 MHz, DMSO-d6) δ 6.95 (s, 4H), 2.90 (d, J=6.0 Hz, 4H), 2.83 (d, J=6.3 Hz, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865718B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-d731ef372b504249a8182a6dcfe22a2c |
| 出典メモ | uspto-grants-2014_10 |