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Triphenylphosphine → Methyl 2-{4-[(tert-butoxycarbonyl)amino]butoxy}-6-hydroxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Methyl 2,6-dihydroxybenzoate | HCID 519869 | — |
| 反応物 | tert-Butyl N-(4-hydroxybutyl)carbamate | HCID 545141 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 2-{4-[(tert-butoxycarbonyl)amino]butoxy}-6-hydroxybenzoate | HCID 10980693 | — |
反応手順
To a solution of methyl 2,6-dihydroxybenzoate (1.0 g, 5.95 mmol) and 4-(Boc-amino)-1-butanol (1.1 mL, 5.95 mmol) in 60 mL of THF is added PPh3 (1.7 g, 6.5 mmol) and DEAD (2.97 mL, 6.5 mmol). The solution is stirred at RT for 18 h then the solvent is removed under reduced pressure. The residue is purified by flash chromatography using a gradient of hexane/EtOAc (5:1 to 2:1) to give the product as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08252820B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-cd05ecbb491847059ab2dc8b69449f5a |
| 出典メモ | uspto-grants-2012_08 |