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Ethyl diazoacetate → (3-Trifluoromethylbenzyloxy)acetic Acid Ethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl diazoacetate | HCID 12192 | — |
| 反応物 | 3-(Trifluoromethyl)benzylic alcohol | HCID 67681 | — |
| 触媒 | Acetic acid, rhodium salt (4:2) | HCID 423677 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | (3-Trifluoromethylbenzyloxy)acetic Acid Ethyl Ester | HCID 68572230 | 97.9% |
反応手順
To a solution of 3-trifluoromethylbenzyl alcohol (1.62 g, 10.0 mmol) in dichloromethane (20 mL) is added rhodium (II) acetate dimer (10 mg) followed by ethyl diazoacetate (0.95 mL, 9.0 mmol). The reaction mixture is stirred at RT for 30 min. The reaction mixture is diluted with heptane, filtered through Celite, and the filtrate is evaporated and the residue is vacuum distilled at 150° C. to give 2.31 g of the product 394. 1H NMR (CDCl3) δ 7.65 (bs, 1H), 7.57 (m, 2H), 7.48 (t, 1H), 4.69 (s, 2H), 4.24 (q, 2H), 4.14 (s, 2H), 1.30 (t, 3H); MS: m/z 263 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741493B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-4849db3f64cf446ca8fa05063e74d175 |
| 出典メモ | uspto-grants-2010_06 |