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p-Chlorothiophenol → 1-Chloro-4-[(2,2-dimethoxyethyl)sulfanyl]benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Chlorothiophenol | HCID 7815 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Bromo-1,1-dimethoxyethane | HCID 81672 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Chloro-4-[(2,2-dimethoxyethyl)sulfanyl]benzene | HCID 14175759 | 98% |
反応手順
To a solution of 4-chlorobenzenethiol (5.78 g; 40 mmol) in anhydrous acetone (50 mL) was added potassium carbonate (5.52 g, 40 mmol) and dropwise at room temperature 2-bromo-1,1-dimethoxy-ethane (4.7 mL, 40 mmol). After 24 h of stirring, the precipitate was filtered, the filtrate concentrated, the residue diluted with water and diethyl ether (150 mL), the organic layer washed successively with water (60 mL), NaOH 4N (30 mL) and water (60 mL), dried over Na2SO4 and concentrated to give 1-chloro-4-(2,2-dimethoxy-ethylsulfanyl)-benzene (compound PRE9) (9.12 g; orange oil) (Yield=98%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07981907B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-e36ba42ae7cd4ffeb7acd3840feff86b |
| 出典メモ | uspto-grants-2011_07 |