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Diethyl Ether → O-3-methoxy-5-methylphenyl dimethylcarbamothioate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | Dimethylthiocarbamoyl chloride | HCID 27871 | — |
| 反応物 | 3-Methoxy-5-Methylphenol | HCID 76674 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | O-3-methoxy-5-methylphenyl dimethylcarbamothioate | HCID 58294848 | 91.5% |
反応手順
To a mixture of 3-methoxy-5-methylphenol (7) (3.39 g, 24.5 mmol) and 1,4-diazabicyclo[2.2.2]octane (5.50 g, 49.0 mmol) in DMF (20 mL) was added dimethylthiocarbamoyl chloride (8) (6.06 g, 49.0 mmol) portionwise. The reaction mixture was stirred at room temperature overnight and 500 mL of ether was added. The organics were washed with water (150 mL), brine (2×50 mL), dried (Na2SO4), and concentrated. Purification by chromatography on silica gel (Hexanes/EtOAc, 4:1) gave O-3-methoxy-5-methylphenyl dimethylcarbamothioate (9) (5.05 g, 91%) as a colourless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08101605B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-3123dddee2e9461a81930c4e3de5ee81 |
| 出典メモ | uspto-grants-2012_01 |