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Diethyl Ether → (R)-2-azido-1-benzylethylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | 1-azido-2-(R)-(BOC-amino)-3-phenylpropane | HCID 22941732 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (R)-2-azido-1-benzylethylamine | HCID 14802497 | 78.9% |
反応手順
The compound from step 164c (4.3 g,15.6 mmol) was dissolved in 30 mL of 4 N HCl in ethanol, and the reaction mixture was stirred for 1.5 hours at room temperature. The solvent was stripped and chased with ether. The residue was dissolved in water, NaCl was added, and the mixture was extracted with ethyl ether, which was discarded. The aqueous layer was adjusted to pH 12 with K2CO3, saturated with NaCl, then extracted with CHCl3. The organic extract was washed with brine, dried (Na2SO4) and filtered. The solvent was removed under vacuum to afford 2.17 g of the title compound. MS m/z (M+H)+ : 177, MS m/z (M+NH4)+ : 194.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06028181 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-5110a25f19e447f08d9f70b9a05a7185 |
| 出典メモ | uspto-grants-2000_02 |