化工社化工社 化学情報印刷レポート · 研究参考用
Water → Cyclohexoxyacetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Cyclohexanol | HCID 7966 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Cyclohexoxyacetic acid | HCID 191994 | 31.7% |
反応手順
To a solution of compound NaH (719 mg, 29.94 mmol) in DMF (10 mL) was added cyclohexanol (1 g, 9.98 mmol) at 0° C. After stirring for 5 minutes, ethyl 2-bromoacetate (2 g, 11.98 mmol) was added and the mixture stirred for another 16 h. Once complete, the mixture was treated with water (50 mL) and washed with ethyl acetate (2×20 mL). The water layer was treat with 2N HCL until pH 3. The water layer was extracted with ethyl acetate (2×20 ml) and the combined organic layers washed with brine (30 mL), dried over Na2SO4 and concentrated to give the desired product (500 mg, 27.8%) as colorless oil which was used in next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08940726B2 |
| 出典データセット | uspto-grants-2015_01 |
| ORD ID | ord-3b552c876dff45edb98b70decfbfa6a1 |
| 出典メモ | uspto-grants-2015_01 |