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Triphenylphosphine → 2-(R)-[2-(N,N-Dimethylamino)ethy]-6-(4-[(4-methoxyphenyl)carbonyloxy]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 | 2-(R)-[2-(N,N-dimethylamino)ethyl]-6-hydroxytetralin | HCID 9964511 | — |
| 反応物 | 4-(Hydroxymethyl)phenyl 4-methoxybenzoate | HCID 21940070 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(R)-[2-(N,N-Dimethylamino)ethy]-6-(4-[(4-methoxyphenyl)carbonyloxy]benzyloxy)tetralin | HCID 58715118 | 50.9% |
反応手順
Diethyl azodicarboxylate (40% toluene solution, 0.95 g) was added dropwise to THF solution (6 ml) of 2-(R)-[2-(N,N-dimethylamino)ethyl]-6-hydroxytetralin (300 mg), 4-(hydroxymethyl)phenyl 4-methoxybenzoate (530 mg), and triphenylphosphine (430 mg) under ice-cooling. After stirring for 2 hours at room temperature, the reaction mixture was concentrated. The residue was purified using alumina column chromatography (development solvent; hexane˜hexane:ethyl acetate=10:1), and the titled compound (320 mg) was obtained after recrystallization (ethyl acetate-hexane).
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-eec9e17bd9214b2a983e8fef5d333989 |
| 出典メモ | uspto-grants-2006_10 |