化工社化工社 化学情報印刷レポート · 研究参考用
4-Aminophenol → tert-Butyl 3-amino-4-hydroxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminophenol | HCID 403 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Di-tert-butyl dicarbonate | HCID 90495 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | tert-Butyl 3-amino-4-hydroxybenzoate | HCID 11160103 | 96.1% |
反応手順
To a solution of 4-aminophenol (10.9 g, 100 mmol) in THF (150 mL) cooled in an ice bath was added di-tert-butyl-dicarbonate (21.8 g, 100 mmol) followed by diisopropylethylamine (17.4 mL, 100 mmol). The mixture was stirred at room temperature overnight and concentrated. The residue was taken up in ethyl acetate and the solution was washed with brine, dried (MgSO4), and concentrated. Purification on a silica gel column eluting with 5% methanol/40% ethyl acetate hexane gave 4Boc-aminophenol (20.1 g, 96%). MS(NH3—CI): (M+NH3+H)=227.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858626B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-a263a6c6aab24b52ae051db78b79b634 |
| 出典メモ | uspto-grants-2005_02 |