関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Propylguaiacol | HCID 17739 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Methoxy-4-propylphenyl 4-methylbenzenesulfonate | HCID 59191389 | 66% |
反応手順
To a solution of 2-methoxy-4-propylphenol (10.0 mmol; 1.6 mL), NaI (1.0 mmol; 150 mg), and K2CO3 (11.0 mmol; 1.52 g), under argon, in acetonitrile (20 mL) was added tosyl chloride (10.5 mmol; 2.0 g). The reaction mixture was stirred at 70° C. for 36 hr, then quenched with NaOH (0.1N; 3 mL), and extracted with ethyl acetate (2*10 mL). Combined organic phases were washed with saturated NaHCO3 sat. (5 mL), dried over MgSO4, concentrated in vacuo. The crude was chromatographed on silica gel (gradient cyclohexane/dichloromethane) to yield the desired compound as a clear oil (2.13 g; 6.6 mmol; 66%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09309179B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-3cc95fae80bc4f42afe4dcfdc47233ef |
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| 出典メモ | uspto-grants-2016_04 |
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