関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Methylbenzylamine | HCID 66035 | — |
| 反応物 | 3-[3-(3-Bromo-propoxy)phenyl]-thieno[2,3-d]isoxazole | HCID 21983559 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (4-Methyl-benzyl)-[3-(3-thieno[2,3-d]isoxazol-3-yl-phenoxy)-propyl]-amine | HCID 21983594 | 80% |
反応手順
Mix 3-[3-(3-bromo-propoxy)-phenyl]-thieno[2,3-d]isoxazole (0.400 g, 1.18 mmol), potassium carbonate (0.326 g, 2.36 mmol), 4-methylbenzylamine (0.606, 5.00 mmol) and acetonitrile (5.0 mL) and heat (75° 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. Dissolved residue in 50% ethyl acetate in dichloromethane and chromatograph on silica (10 g) using ethyl acetate to give the title compound (356 mg, 80% yield). Purity by LC/MS (APCI)=98, [M+H]+=379.
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-a99c1c0c4a2345f79a71dc7c55462a97 |
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| 出典メモ | uspto-grants-2006_08 |
|---|
