関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Methoxybenzylamine | HCID 81292 | — |
| 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-Methoxy-benzyl)-[2-(3-thieno[2,3-d]isoxazol-3-yl-phenoxy)-ethyl]-amine | HCID 21983563 | 90% |
反応手順
Mix 3-[3-(2-bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole (0.324 g, 1 mmol), potassium carbonate (0.28 g, 2 mmol), 2-methoxybenzylamine (0.686 g, 5 mmol) and acetonitrile (anhydrous, 4 mL) and heat at 75° C. for 16.5 hours. Cool the reaction mixture and filter through a Waters Sep-Pak silica gel cartridge (1 g) using ethyl acetate. Combine the appropriate fractions and concentrate to give a residue. Purify the residue by column (10 g silica) chromatography using a step gradient of 60% ethyl acetate in heptane to 100% ethyl acetate to give the title compound (342 mg, 90% Yield). Purity by LC/MS (APCI)=99%, [M+H]+=381.
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-7a23060077fa4a118beecc9e547f6e26 |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|