化工社化工社 化学情報印刷レポート · 研究参考用
Water → 6-Chloro-2-fluoro-3-(2,2,2-trifluoro-ethoxy)-benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Chloro-2-fluoro-1-(2,2,2-trifluoroethoxy)benzene | HCID 59506748 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Acetone cardice | HCID 18522661 | — |
| 生成物 | 6-Chloro-2-fluoro-3-(2,2,2-trifluoro-ethoxy)-benzaldehyde | HCID 59506829 | — |
反応手順
To 4-Chloro-2-fluoro-1-(2,2,2-trifluoro-ethoxy)-benzene (522, 0.80 g, 3.5 mmol) in THF (20 mL), cooled in dry ice/acetone bath and under an atmosphere of nitrogen, was slowly added n-butyllithium (1.60 M in Hexane, 2.30 mL). After an hour, N,N-dimethylformamide (0.298 mL, 3.85 mmol) was added to the reaction. After 30 minutes, the reaction was allowed to reach room temperature and was stirred for 10 minutes. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 20% ethyl acetate in hexane to give the compound (523, 450 mg, 50%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863288B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-22949da1191b41feaab46b63d8d4a5de |
| 出典メモ | uspto-grants-2011_01 |