化工社化工社 化学情報印刷レポート · 研究参考用
Lithium Hydroxide → 2-Ethoxy-4-(trifluoromethyl)benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Ethyl 2-ethoxy-4-(trifluoromethyl)benzoate | HCID 66857656 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Ethoxy-4-(trifluoromethyl)benzoic acid | HCID 22494327 | 88% |
反応手順
2-Hydroxy-4-trifluoromethyl-benzoic acid (1.20 g, 5.82 mmol) was reacted with ethyliodide (2.2 eq) and K2CO3 (1.69 g) in DMF solution. The reaction mixture was quenched by adding H2O. The mixture was extracted with ethyl acetate (40 ml×3). A combined organic layer was washed sat NaHCO3 solution (30 ml), H2O (40 ml×5), and brine, and then dried over MgSO4. The filterate was concentrated in vacuo to yield 2-ethoxy-4-trifluoromethyl benzoic acid ethyl ester. The ester obtained above was reacted with 1 N LiOH (15 ml) in THF and CH3OH cosolvent for 2 hrs as described above to yield title compound (1.20 g, 88%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08557872B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-8a1f172a9cbe401b91b5ef256879c430 |
| 出典メモ | uspto-grants-2013_10 |