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Triethylamine → N-(2-bromo-5-methylphenyl)cyclopropanecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| 反応物 | 2-Bromo-5-methylaniline | HCID 6422065 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | N-(2-bromo-5-methylphenyl)cyclopropanecarboxamide | HCID 68501761 | — |
反応手順
The solution of 13.95 g of 2-bromo-5-methylphenylamine in 250 ml of chloroform is cooled to 0° C. with stirring and admixed with 12.6 ml of triethylamine. 7.56 ml of cyclopropanecarbonyl chloride are slowly added dropwise. The mixture is stirred for 1 hour each at 0° C. and at room temperature. The reaction mixture is poured onto water (400 ml) and extracted with dichloromethane (1×250 ml). The organic phases are washed with brine (350 ml), dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a white solid from the residue by means of crystallization from ethyl acetate. Rf=0.37 (1:4 EtOAc-heptane); Rt=4.19.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07842688B2 |
| 出典データセット | uspto-grants-2010_11 |
| ORD ID | ord-ae3402443c47488db131d8b3655409e6 |
| 出典メモ | uspto-grants-2010_11 |