関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | 2-Bromoethanol | HCID 10898 | — |
| 反応物 | 4-Amino-1,2,4-triazole | HCID 11432 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178475127 | HCID 178475127 | — |
反応手順
5.000 grams, 59.4 mmoles of 4-amino-1,2,4-triazole was dissolved in 200 ml of fresh acetonitrile and stirred vigorously. 29.800 grams of 2-bromoethanol was added slowly to the solution by pipet. After the addition was complete, the reaction mixture was heated for 20 hours at 80° C., until thin layer chromatography revealed that all of the 4-amino-1,2,4-triazole had been consumed. The reaction mixture was then allowed to cool to room temperature and then was rotary evaporated down to leave a viscous oil. Hot isopropyl alcohol was added to the oil dissolving it. Storage of the resultant solution in a refrigerator resulting in a large crop of a viscous oil of 1-ethanol-4-amino-1,2,4-triazolium bromide, 9.9332 g, 47.5 mmoles. Melting point 0-5° C.; DSC onset 180° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07745635B1 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-636d9b24fc2f447daf8cdd76a40f5893 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|