化工社化工社 化学情報印刷レポート · 研究参考用
Sodium hydride → 2-Cyclopropylmethoxy-4-fluoro-1-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| 反応物 | Cyclopropanemethanol | HCID 75644 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Cyclopropylmethoxy-4-fluoro-1-nitrobenzene | HCID 58998409 | 86% |
反応手順
Cyclopropyl methanol (15 g, 207 mmol) was added to a stirred suspension of NaH (60% in mineral oil, 8.37 g) in 200 mL THF over a period of 15 min at 0° C. under an atmosphere of nitrogen. The reaction mixture was allowed to warm to room temperature and stirred for 1 h at RT. The mixture was cooled to 0° C. and a solution of 2,4-difluoro-1-nitrobenzene (30 g, 187 mmol) in 200 mL THF was added in a drop wise manner. The reaction mixture was stirred at 0° C. for 2 h and then poured onto ice water. The mixture was extracted with ethyl acetate (3×100 mL). The combined organic layers were dried over MgSO4 and concentrated under reduced pressure to give 22.0 g of 2-(cyclopropylmethoxy)-4-fluoro-1-nitrobenzene as an orange oil (86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367863B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-6751e940abe7427bbd484164ac6b6a6d |
| 出典メモ | uspto-grants-2013_02 |