참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Butylated Hydroxyanisole | HCID 8456 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dimethyl Carbonate | HCID 12021 | — |
| 생성물 | 2-Tert-butyl-4-methoxyphenyl methanesulfonate | HCID 86668285 | 76% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09029024B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-e6cb5f084f1e46d0a94f4f047535c050 |
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| 출처 메모 | uspto-grants-2015_05 |
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