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Trifluoromethanesulfonic acid → N-trifluoroacetyl-2-iodo-4-chlorophenethylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoromethanesulfonic acid | HCID 62406 | — |
| 反応物 | Bis(pyridine)iodonium tetrafluoroborate | HCID 10883201 | — |
| 反応物 | n-Trifluoroacetyl-4-chlorophenethylamine | HCID 22292794 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-trifluoroacetyl-2-iodo-4-chlorophenethylamine | HCID 22292821 | 38.9% |
反応手順
A solution of N-trifluoroacetyl-4-chlorophenethylamine (1.6 g, 6.4 mmol) in dichloromethane (20 mL) was treated with bis(pyridine)iodonium(I)tetrafluoroborate (2.6 g, 7.0 mmol), CF3SO3H (2.1 g, 14.1 mmol) and stirred overnight at 20 C. The product mixture was concentrated, dissolved in EtOAc (100 mL), washed twice with 5% aqueous sodium bisulfite (50 mL), twice with saturated aqueous NaHCO3, (50 mL) once with brine (50 mL), dried with Na2SO4 and concentrated to give 0.94 g of a clear oil. MS calculated for C10H8ClF3INO+H: 378, observed: 378.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846906B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-cec1420d753248ff8235aef281b7638e |
| 出典メモ | uspto-grants-2014_09 |