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Hydrochloric Acid → 2-(4-((4-(4-Amino-2-bromophenoxy)piperidin-1-yl)methyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-(4-((4-(2-Bromo-4-nitrophenoxy)piperidin-1-yl)methyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol | HCID 86670932 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-((4-(4-Amino-2-bromophenoxy)piperidin-1-yl)methyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol | HCID 86670933 | 90.8% |
反応手順
Iron (94 mmol, 5.24 g) (reduced powder) was added to a suspension 2-(4-((4-(2-bromo-4-nitrophenoxy)piperidin-1-yl)methyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (9.40 mmol, 5.24 g) in 2-propanol (100 mL) containing concentrated hydrochloric acid (1 mL) and the mixture refluxed for 4.5 hours. The mixture was cooled, diluted with dichloromethane and filtered through dicalite. The filtrate was washed with sodium carbonate solution, the organic phase dried over magnesium sulfate and concentrated under reduced pressure to afford the title compound (4.5 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108939B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-19422ed402314bf1a53197ff99adffdb |
| 出典メモ | uspto-grants-2015_08 |