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-(2-Bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole | HCID 21983582 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (2-Fluoro-benzyl)-[2-(3-thieno[2,3-d]isoxazol-3-yl-phenoxy)-ethyl]-amine | HCID 21983592 | 83.4% |
反応手順
Mix 3-[3-(2-bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole (0.40 g, 1.23 mmol), potassium carbonate (0.341 g, 2.47 mmol), 2-fluorobenzylamine (0.626 g, 5.0 mmol) and acetonitrile (5.0 mL) and heat at 80° C., overnight. Cool the reaction mixture and filter through a Waters Sep-Pak 1 g silica cartridge (ethyl acetate). Combine the appropriate fractions and concentrate to give a residue. Purify the residue by column (10 g silica) chromatography using a solvent gradient of 40% ethyl acetate in heptane to 100% ethyl acetate to obtain the title compound (0.378 g, 83% Yield). Purity by LC/MS (APCI)=99%, [M+H]+=369.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07091199B1 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-4538b46408a348e9ba852736e080caa3 |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|