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Nitrogen → 3-(4-Hydroxybutyl)-1,8,8-trimethyl-3-azabicyclo-[3.2.1]octane-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 4-Amino-1-butanol | HCID 25868 | — |
| 反応物 | 1,8,8-Trimethyl-3-oxabicyclo[3.2.1]octane-2,4-dione | HCID 94834 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(4-Hydroxybutyl)-1,8,8-trimethyl-3-azabicyclo-[3.2.1]octane-2,4-dione | HCID 14649067 | — |
反応手順
To a 125 ml round-bottomed flask equipped with Dean-Stark trap, condenser, and N2 inlet were added 5.35 g (29 mmol) of d-camphoric anhydride, 2.49 g (28 mmol) of 4-hydroxybutylamine, and 60 ml of toluene. The reaction was refluxed with separation of water for 20 hours. It was then cooled, concentrated to an oil, and the oil dissolved in ethyl acetate. The ethyl acetate solution was washed with 5% HCl, 5% NaOH, and brine, dried over sodium sulfate, and evaporated to an oil, 6.0 g (85%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05077295 |
| 出典データセット | uspto-grants-1991_12 |
| ORD ID | ord-f235a3e4cf324df5b44a3d694eb1d139 |
| 出典メモ | uspto-grants-1991_12 |