関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Acetylcyclohexanone | HCID 13400 | — |
| 反応物 | HCID 178508559 | HCID 178508559 | — |
| 溶媒 | 2-Methoxyethanol | HCID 8019 | — |
| 生成物 | (5-Methyl-6,7,8,9-tetrahydro-[1,2,4]triazolo[1,5-a]quinazolin-2-yl)-methanol | HCID 22224538 | 50.8% |
反応手順
To a round bottomed flask was loaded 4.2 grams of 2-acetylcyclohexanone, 3.52 grams of (5-Amino-1H-[1,2,4]triazol-3-yl)-methanol and 50 ml 2-methoxyethanol. The mixture was refluxed for 18 hours. Then it was cooled down to 23° C. and concentrated to 5 ml. Then 50 ml ethyl ether was added and the precipitate was filtered and vacuum dried to yielded 3.32 grams of product Yield. 49%. This compound was used directly for the next step. MS: 219.2 (M+H). H-NMR (DMSO): δ 5.49 (t, 1H, OH, J=6 Hz), 4.61 (d, 2H, J=6 Hz), 3.24 (m, 2H), 2.93 (m, 2H), 2.69 (s, 3H), 2.52 (s, 2H), 1.84 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07691842B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-9dd6135df5004ceca91ecfd8d7823ffd |
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| 出典メモ | uspto-grants-2010_04 |
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