化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Cyanide → 5-nitro-3-pyridin-2-yl-3,4-dihydro-2H-1,4-benzoxazine-3-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | 5-nitro-3-pyridin-2-yl-2H-1,4-benzoxazine | HCID 90408902 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-nitro-3-pyridin-2-yl-3,4-dihydro-2H-1,4-benzoxazine-3-carbonitrile | HCID 90410150 | — |
反応手順
Potassium cyanide (500 mg, 7 mmol) was added to a solution of 5-nitro-3-pyridin-2-yl-2H-1,4-benzoxazine (1 g, 4 mmol) (Example 70, Step 1), in acetonitrile (20 mL), and was stirred overnight at room temperature. The reaction was partitioned between ethyl acetate and water, and the organic layer was washed with brine, dried over magnesium sulfate, filtered, and concentrated to give the crude product. The product was crystallized from methylene chloride to give 5-nitro-3-pyridin-2-yl-3,4-dihydro-2H-1,4-benzoxazine-3-carbonitrile as a dark yellow powder (0.60 g. 60%). LCMS calculated for C14H11N4O3 (M+H)+: m/z=283.1. found: 282.9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09227985B2 |
| 出典データセット | uspto-grants-2016_01 |
| ORD ID | ord-b904f1080dd840b5b8c47410b86b2b8d |
| 出典メモ | uspto-grants-2016_01 |