関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 5-Bromo-2-fluoro-1,3-dimethylbenzene | HCID 2736298 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 5-Bromo-1,3-dimethyl-2-(methylsulfanyl)benzene | HCID 68519501 | 14.2% |
反応手順
Add 5-bromo-2-fluoro-1,3-dimethyl-benzene (3.5 g, 17.2 mmol) to dimethylformamide (DMF, 30 mL) at ambient temperature followed by sodium thiomethoxide (1.32 g, 17.9 mmol). Heat at 50° C. for 8 hours and dilute with water (10 mL) and diethyl ether (100 mL). Separate the layers, wash the organics with brine, and dry with magnesium sulfate before concentrating to a residue. Chromatograph the residue on a SiO2 column eluting with diethyl ether (20%) in hexane to give 566 mg (14%) of 5-bromo-1,3-dimethyl-2-methylsulfanyl-benzene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07585977B2 |
|---|
| 出典データセット | uspto-grants-2009_09 |
|---|
| ORD ID | ord-13edda37ddd44583938f634527cac803 |
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| 出典メモ | uspto-grants-2009_09 |
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