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Triphenylphosphine → HCID 21939854、化合物
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 | 2-(N,N-Dimethylamino)methyl-6-hydroxytetralin | HCID 21939764 | — |
| 反応物 | 4-(Hydroxymethyl)phenyl 4-methoxybenzoate | HCID 21940070 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 21939854 | HCID 21939854 | 53.8% |
反応手順
Diethyl azodicarboxylate (40% toluene solution, 950 mg) was added dropwise to THF solution (3 ml) of 2-[(N,N-dimethylamino)methyl]-6-hydroxytetralin (150 mg), 4-(hydroxymethyl)phenyl 4-methoxybenzoate (570 mg) and triphenylphosphine (574 mg) at room temperature, which was stirred for 3 hours. The reaction mixture was concentrated, and the residue was purified using alumina column chromatography (development solvent; hexane˜hexane:ethyl acetate=6:1), and recrystallized (ethyl acetate-hexane) to give the titled compound (175 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-3bb54d2b3b8547e8adcb154f5c2e16b6 |
| 出典メモ | uspto-grants-2006_10 |