関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Decanethiol | HCID 8917 | — |
| 反応物 | 11-Bromoundecanoic acid | HCID 17812 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178442874 | HCID 178442874 | 82.4% |
反応手順
In a 3000 ml flask equipped with a stirrer and a condenser were charged 132 g of 11-bromoundecanoic acid, 91.5 g of n-decanthiol, 59.4 g of sodium methoxide (28% methanol solution) and 1500 ml of methanol, and the mixture was refluxed for 12 hours. After completion of the reaction, the reaction mixture was cooled to room temperature, precipitated crystals were collected by filtration under reduced pressure and the resulting crystals were washed with methanol. The resulting crystals were suspended in 5000 ml of distilled water, and the suspension was neutralized by a conc. hydrochloric acid, and the crystals were again collected by filtration under reduced pressure. The crystals were washed with water until the washed solution became neutral, and recrystallized from ethanol to obtain 140.5 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06184180B2 |
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| 出典データセット | uspto-grants-2001_02 |
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| ORD ID | ord-89ee4cff4ea841b6b3a3a1ee7cc50dff |
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| 出典メモ | uspto-grants-2001_02 |
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