関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phthalimide | HCID 6809 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | [2-(4-dipropylaminobutyl)-3-propyl-3H-benzimidazol-5-yl]methanol | HCID 23079221 | — |
| 反応物 | Diethylazodicarboxylate toluene | HCID 66777355 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-[2-(4-dipropylaminobutyl)-3-propyl-3H-benzimidazol-5-ylmethyl]isoindole-1,3-dione | HCID 23155501 | 41.9% |
反応手順
The compound (302 mg) obtained in Example 125-4 was dissolved in toluene (6.0 ml) and added with triphenylphosphine (275 mg) and phthalimide (193 mg), followed by cooling to 0° C. In this solution, a 40% diethyl azodicarboxylate/toluene solution (452 mg) was dropped. After that, the solution was stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in chloroform and washed with water. Then, the solution was subjected to extraction with chloroform and the extract was then washed with saturated saline solution. The organic layer was dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure and the residue was then purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (174 mg) as a pale-yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07176227B2 |
|---|
| 出典データセット | uspto-grants-2007_02 |
|---|
| ORD ID | ord-b38b06ee95044a93b17e6cf98e20a304 |
|---|
| 出典メモ | uspto-grants-2007_02 |
|---|