참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Butene, 1-bromo-3-methyl- | HCID 70092 | — |
| 반응물 | 3-Methoxybenzenethiol | HCID 84989 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 1-Methoxy-3-(3-methylbut-2-enylsulphanyl)benzene | HCID 22592592 | 90.4% |
반응 단계
50.45 g (360.0 mmol) of 3-methoxythiophenol, 360 ml of acetone and 14.40 g (360.0 mmol) of sodium hydroxide pellets are introduced into a one liter round-bottomed flask under a nitrogen atmosphere and the mixture is heated at reflux for three hours. A solution composed of 53.6 g (360.0 mmol) of 2-methyl-4-bromo-2-butene and of 60 ml of acetone is added dropwise. Reflux is maintained for sixteen hours and the reaction mixture is evaporated to dryness. Water is added, extraction is carried out with ethyl acetate, the organic phase is washed with water and then using a saturated sodium chloride solution, dried over magnesium sulphate and filtered, and the solvents are evaporated. The residue obtained is distilled under reduced pressure (5×10−2 bar/113° C.) to produce 67.81 g (90%) of the expected compound in the form or a pale-yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06849658B2 |
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| 출처 데이터셋 | uspto-grants-2005_02 |
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| ORD ID | ord-b12277d88d5544d0af86d992556ac845 |
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| 출처 메모 | uspto-grants-2005_02 |
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