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Chloroform → 3-Bromo-2,6-dimethylbenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2,6-Dimethylbenzonitrile | HCID 81057 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Bromo-2,6-dimethylbenzonitrile | HCID 21199122 | — |
反応手順
A mixture of 2,6-dimethylbenzonitrile (5.0 g, 38.0 mmol), bromine (1.9 ml, 38.0 mmol) and chloroform (10 ml) is stirred at room temperature for 24 hours and subsequently heated to 60° C. for 6 hours. Upon cooling down to 0° C., 10 g of AlCl3 are added and the mixture is stirred for 4 hours at 0° C. The reaction mixture is poured into water and extracted with toluene. The organic phase is separated and concentrated and the residue is purified by column chromatography yielding the pure product as brown crystals, 6.2 g, mp. 60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06242498B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-c743b4deb59541ecad943013fd7950f7 |
| 出典メモ | uspto-grants-2001_06 |