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Propanoic acid, 2-bromo-2-methyl-, ethyl ester → 2-Cyclohexylsulfanyl-2-methyl-propionic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Propanoic acid, 2-bromo-2-methyl-, ethyl ester | HCID 11745 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Cyclohexanethiol | HCID 15290 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Cyclohexylsulfanyl-2-methyl-propionic acid ethyl ester | HCID 21397848 | 83.8% |
反応手順
To a solution of 2.5 g (21.5 mmol) of cyclohexyl thiol in ethanol (75 mL) were added 1.2 g (21.5 mmol) of KOH pellets, followed by 4.2 g (21.5 mmol) of ethyl α-bromoisobutyrate. The reaction was heated to reflux for 18 h and then cooled to room temperature. The solid (KBr) was separated by filtration and rinsed with ethanol (20 mL). The filtrate was concentrated under reduced pressure and the residue dissolved in DCM (50 mL). The organic layer was washed with water (2×20 mL). The aqueous washes were back-extracted with DCM (10 mL). The combined organics were washed with brine, dried over Na2SO4. Filtration and concentration under reduced pressure afforded 4.15 g of 2-cyclohexylsulfanyl-2-methyl-propionic acid ethyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829034B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-292c8a712f114a24824ba6932dd5b182 |
| 出典メモ | uspto-grants-2014_09 |