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Imidazole → 3-(Tert-butyldiphenylsilyloxy)butan-1-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | 1-Amino-2-butanol | HCID 26107 | — |
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(Tert-butyldiphenylsilyloxy)butan-1-amine | HCID 58842027 | 181.5% |
反応手順
To a solution of 2-hydroxybutylamine (4.00 g, 44.87 mmol) in anhydrous DMF (25 mL) was added tert-butyldiphenylsilylchloride (16.9 mL, 66.19 mmol) and imidazole (9.16 g, 13.46 mmol). The reaction mixture was stirred at room temperature for 2 days, then concentrated under reduced pressure, and diluted with CH2Cl2 (150 mL). The organics were washed with 5% aqueous NaHCO3 solution (50 mL), brine (50 mL), dried (MgSO4), filtered, and concentrated. The crude material was purified by column chromatography (0 to 100% EtOAc in hexane) to give 3-(tert-butyldiphenylsilyloxy)butan-1-amine (8.00 g, 54%) as a white solid. 1H NMR and MS consistent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863271B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-f5b564884e16498d909f4bcd7ddd4f55 |
| 出典メモ | uspto-grants-2011_01 |