化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → HCID 178434636、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Hydrazine, dihydrochloride | HCID 17548 | — |
| 反応物 | 2-(8-Fluoro-2,3-dihydro-1,4-benzodioxin-6-yl)-3-oxobutanenitrile | HCID 66891603 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178434636 | HCID 178434636 | 93% |
反応手順
2-(8-fluoro-2,3-dihydro-1,4-benzodioxin-6-yl)-3-oxobutanenitrile (0.37 g; 1.56 mmol) was dissolved in dry ethanol (5 mL) and hydrazine dihydrochloride (0.20 g, 1.87 mmol) then triethylamine (217 μg, 1.56 mmol) were added. The reaction mixture was refluxed for 2 h, cooled to rt and the solvent was evaporated under vacuum. The residue was dissolved in ethyl acetate (50 ml), washed with saturated sodium bicarbonate (2×25 mL), brine (25 ml) then dried over sodium sulfate. Filtration and concentration gave 4-(8-fluoro-2,3-dihydro-1,4-benzodioxin-6-yl)-3-methyl-1H-pyrazol-5-amine (0.36 g, 93% yield) as an orange solid. 1H NMR (400 MHz, d6-DMSO) δ 6.75 (dd, 1H), 6.65 (m, 1H), 4.30 (m, 4H), 2.14 (s, 3H). MS (EI) for C12H12FN3O2: 250 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07872014B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-2ab85eabb79246c9b87bc937062b31b8 |
| 出典メモ | uspto-grants-2011_01 |