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Triphenylphosphine → 2-[(N,N-Dimethylamino)methyl]-6-[4-[(4-methoxybenzyl)oxy]benzyloxy]tetralin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 反応物 | 4-[(4-Methoxyphenyl)methoxy]benzenemethanol | HCID 12648421 | — |
| 反応物 | 2-(N,N-Dimethylamino)methyl-6-hydroxytetralin | HCID 21939764 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[(N,N-Dimethylamino)methyl]-6-[4-[(4-methoxybenzyl)oxy]benzyloxy]tetralin | HCID 21940053 | 41.2% |
反応手順
Diethyl azodicarboxylate (40% toluene solution, 1.91 g) was added dropwise to THF solution (6 ml) of 2-[(N,N-dimethylamino)methyl]-6-hydroxytetralin (300 mg), 4-[(4-methoxybenzyl)oxy]benzylalcohol (1.07 g) and triphenylphosphine (1.15 g) at room temperature, which was stirred for 12 hours. The reaction mixture was concentrated, and the residue was purified using alumina column chromatography (development solvent; hexane˜hexane:ethyl acetate=10:1), and recrystallized (ethyl acetate-hexane) to give the titled compound (260 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07115750B1 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-037b1f8e563c4a369842696cc76cff45 |
| 出典メモ | uspto-grants-2006_10 |