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Thionyl Chloride → N-(2-hydroxy-6-methylphenyl)-2-bromo-5-methyl-3-thiophenecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 2-Amino-m-cresol | HCID 3014138 | — |
| 反応物 | 2-Bromo-5-methylthiophene-3-carboxylic acid | HCID 11117589 | — |
| 反応物 | 2-Bromo-5-methyl-3-thiophenecarbonyl chloride | HCID 18422254 | — |
| 反応物 | Diisopropylether ethyl acetate | HCID 22281796 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(2-hydroxy-6-methylphenyl)-2-bromo-5-methyl-3-thiophenecarboxamide | HCID 11110188 | 84.7% |
反応手順
2-Bromo-5-methyl-3-thiophenecarbonyl chloride (2.6 g), prepared in the same manner as above from 2-bromo-5-methyl-3-thiophenecarboxylic acid and thionyl chloride, was suspended in toluene (20 ml). This toluene solution was added dropwise to a solution of 2-amino-3-methylphenol (1.4 g) in pyridine (30 ml) at 0° C. The mixture was stirred at room temperature for 3 hours and diisopropyl ether-ethyl acetate was added. The solvent was evaporated under reduced pressure. The precipitated crystals were collected by filtration, and washed with diluted hydrochloric acid and diisopropyl ether to give N-(2-hydroxy-6-methylphenyl)-2-bromo-5-methyl-3-thiophenecarboxamide (3.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06455521B1 |
| 出典データセット | uspto-grants-2002_09 |
| ORD ID | ord-22940ab0c11f4e49b705d3df759681af |
| 出典メモ | uspto-grants-2002_09 |