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Magnesium chloride hexahydrate → 4-Bromo-2-methylthiobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Magnesium chloride hexahydrate | HCID 24644 | — |
| 反応物 | Sodium hydrosulfide | HCID 28015 | — |
| 反応物 | 4-Bromo-2-methylbenzonitrile | HCID 144267 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Bromo-2-methylthiobenzamide | HCID 45040716 | 7.1% |
反応手順
To a slurry solution of sodium hydrosulphide (2.80 g, 50 mmol) and magnesium chloride hexahydrate (5.05 g, 25 mmol) in dimethylformamide (50 ml) is added 4-bromo-2-methyl benzonitrile (4.90 g, 50 mmol) in one portion and the resulting green slurry is stirred at room temp for 90 minutes. The reaction mixture is poured onto water (200 ml) and the resultant precipitate filtered and washed with water. This yellow solid is then suspended in 2N HCl (200 ml) and stirred for 1 hour, then filtered, washed with water and hexane and dried in vacuo to give 4-bromo-2-methyl-thiobenzamide (820 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530667B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-48bd0dd0b0c445288e15b03541b8230a |
| 出典メモ | uspto-grants-2013_09 |