化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2-N-methyl-6-fluoro-1-isoquinolinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Fluoroisoquinolin-1(2H)-one | HCID 45090802 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-N-methyl-6-fluoro-1-isoquinolinone | HCID 69399976 | 107.5% |
反応手順
Sodium hydride (60% in mineral oil) (211 mg, 5.27 mmol) was added to 6-fluoro-1,2-dihydroisoquinolin-1-one (716 mg, 4.39 mmol) in anhydrous DMF (6 mL) cooled in an ice bath. The mixture was stirred for about 30 min at room temperature and methyl iodide (0.328 mL, 5.27 mmol) was added dropwise. After 1 h, the reaction was judged to be about 60% complete and additional methyl iodide (0.2 mL, 3.2 mmol) was added. After about 1 h, ice and water and ethyl acetate were added to the mixture. After extractive work up with ethyl acetate, the title compound (836 mg) was obtained as a cream solid and carried on without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09034900B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-0e5454cf6fb4431a84ed25aa1fe6640b |
| 出典メモ | uspto-grants-2015_05 |