関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butylated Hydroxyanisole | HCID 8456 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dimethyl Carbonate | HCID 12021 | — |
| 生成物 | 2-Tert-butyl-4-methoxyphenyl methanesulfonate | HCID 86668285 | 76% |
反応手順
15.0 g (83.2 mmol) of 4-hydroxy-3-tert-butylanisole and 10.5 g (104 mmol) of triethylamine were dissolved in 250 ml of dimethyl carbonate (solvent), and 11.9 g (104 mmol) of methanesulfonyl chloride was dropwise added thereto, taking 25 minutes and controlling the inner temperature at 5° C. or lower. After the addition, this was stirred at 25° C. for 1.5 hours, the reaction mixture was poured into an aqueous saturated sodium bicarbonate solution, the aqueous layer was separated, the organic layer was washed twice with water, and then the organic layer was separated and concentrated. The concentrate was purified through distillation (139° C./32 pa) to give 16.3 g of 2-tert-butyl-4-methoxyphenyl methanesulfonate (yield, 76%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09029024B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-e6cb5f084f1e46d0a94f4f047535c050 |
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| 出典メモ | uspto-grants-2015_05 |
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