関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | EDTA disodium salt | HCID 8759 | — |
| 反応物 | (E)-3-Chloro-N-methyl-N-(1-naphthylmethyl)-2-propen-1-amine | HCID 9834733 | — |
| 触媒 | Nickel Dichloride | HCID 24385 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Terbinafine | HCID 1549008 | — |
反応手順
The mixture is cooled to 50° C. and 15.5 g (0.0572 mol) crude N-(trans-3-chloro-2-propenyl)-N-methyl-1-naphthalene-methylamine, 20 ml THF and 74 mg NiCl2 (0.77 molar percent) introduced. The reaction mixture is heated at 90°-95° C. for 1 hour, cooled to 20°/25° C. and 130 ml of a 2.5% (w/v) aqueous solution of EDTA disodium salt added, the phases are separated and the aqueous phase re-extracted with 70 ml chilled toluene. The combined organic phases are washed with 2×90 ml water and concentrated to a residue, thus giving 18.2 g (greater than theoretical yield) terbinafine with a purity of 83.6% (HPLC A %).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07838704B2 |
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| 出典データセット | uspto-grants-2010_11 |
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| ORD ID | ord-f4bb78528cd24f21ac9fcd3b7ec3fc94 |
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| 出典メモ | uspto-grants-2010_11 |
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