関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Ethyl 4-(1,1-dimethylethylsulfinamido)-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate | HCID 86695628 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 4-amino-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate | HCID 69083532 | — |
反応手順
A cooled (0° C.) solution of ethyl 4-(1,1-dimethylethylsulfinamido)-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate (1.550 g; 4.00 mmol) in EtOH (20 ml) was treated dropwise with a solution of 4 M HCl in 1,4-dioxane (2.0 ml; 8.00 mmol). The resulting mixture was further stirred at 0° C., under nitrogen, for 10 min., and then at rt for 30 min. The reaction mixture was then concentrated to dryness under reduced pressure and the oily residue was further dried under HV to give the chlorhydrate salt of ethyl 4-amino-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate. LC-MS (conditions A): tR=0.55 min. and [M+H]+: 284.07 g/mol; tR=0.57 min. and [M+H]+: 284.07 g/mol (mixture of diastereoisomers).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09242970B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-6df2a8f044bb4c0fbd2c67069f1fa547 |
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| 出典メモ | uspto-grants-2016_01 |
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