関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ethyl Bromide | HCID 6332 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Hydroxy-3-methylbenzoic acid | HCID 68138 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 68291767 | HCID 68291767 | — |
反応手順
To a solution of 4-hydroxy-3-methyl-benzoic acid (1.00 g, 6.57 mmol) in N,N-dimethylformamide (10 mL) was added potassium carbonate (2.73 g, 19.7 mmol) and bromoethane (3.58 g, 2.44 mL, 32.9 mmol). The reaction mixture heated at 45° C. for 48 h in a sealed tube. The reaction mixture allowed to cool then diluted with water and ether. The ether layer was washed with 50% saturated NaHCO3 (50 mL) and brine (50 mL), dried over Na2SO4, and concentrated in vacuo to provide ethyl 4-ethoxy-3-methylbenzoate as an orange-colored oil. The crude product was taken directly to the next step. ESI-MS m/z calc. 208.10994. Found 209.3 (M+1)+; Retention time: 1.78 minutes (3 min run).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08828996B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-618f5b7fd05b46789297afc7e800762d |
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| 出典メモ | uspto-grants-2014_09 |
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