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Bromocyclopropane → Butyl-[1-(2-cyclopropyl-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromocyclopropane | HCID 78037 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | Butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine | HCID 58167770 | — |
| 触媒 | Manganese(2+) dichloride | HCID 10313134 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Butyl-[1-(2-cyclopropyl-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine | HCID 58167766 | — |
反応手順
Cyclopropylbromide (3.84 g, 32 mmol) was added to magnesium (771 mg, 32 mmol) in 20 mL diethylether and refluxed for 10 min. Manganese(II) chloride (160 mg, 1.27 mmol) and butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine (intermediate M, 4 g, 13 mmol) was added. The reaction mixture was refluxed for 2 h. The reaction mixture was quenched with 8 mL water and filtered through dicalite. The organic phase was separated and dried on sodium sulfate, filtered and evaporated. The crude material, brown oil (3.54 g, 82%) was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524909B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-98c6ae645cf442be9c235d2382fa39de |
| 出典メモ | uspto-grants-2013_09 |