関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Fluorobenzylamine | HCID 66649 | — |
| 反応物 | 3-[3-(3-Chloro-propoxy)-phenyl]-thieno[2,3-d]isoxazole | HCID 21983556 | — |
| 反応物 | 3-[3-(3-Bromo-propoxy)phenyl]-thieno[2,3-d]isoxazole | HCID 21983559 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | (2-Fluoro-benzyl)-[3-(3-thieno[2,3-d]isoxazol-3-yl-phenoxy)-propyl]-amine | HCID 21983554 | 94.1% |
反応手順
Combine a mixture (1 mmol total) of 3-[3-(3-bromo-propoxy)-phenyl]-thieno[2,3-d]isoxazole, 3-[3-(3-chloro-propoxy)-phenyl]-thieno[2,3-d]isoxazole with 2-fluorobenzylamine (0.63 g, 5.0 mmol), potassium carbonate (0.41 g, 3.0 mmol) and a mixture of acetonitrile:water (80:20) and heat (80° C.) for 30 hours. Cool the reaction mixture and concentrate to give a residue. Purify the residue by column (silica) chromatography (ethyl acetate). Combine the appropriate fractions and concentrate to give the title compound (0.36 g, 94% Yield) as an oil. Purity by LC/MS (APCI)=100% area, [M+H]+=383 g/mol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091199B1 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-7618583492454d46a32c9c9120713d00 |
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| 出典メモ | uspto-grants-2006_08 |
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