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Pyridine → Methyl [2-(4-bromophenyl)-1-methylethyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | 4-Bromo-alpha-methylbenzeneethanamine | HCID 205668 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl [2-(4-bromophenyl)-1-methylethyl]carbamate | HCID 59402313 | — |
反応手順
To a solution of 1-(4-bromophenyl)propan-2-amine (0.5 g, 2 mmol) in methylene chloride (5 mL) was added pyridine (380 uL, 4.7 mmol) and methyl chloroformate (270 uL, 3.5 mmol, Aldrich, Cat. No. M35304). The reaction mixture was stirred at r.t. overnight, and concentrated under reduced pressure. The residue was dissolved in EtOAc, and washed with NaHCO3 aqueous solution, 1N HCl aqueous solution and brine. The organic layer was dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatograph on a silica gel column using 25% Ethyl acetate in hexane to afford the desired compound. LCMS (M+H)+: m/z=272.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08436008B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-e6a0159922a247c797a3839c9ef80c8a |
| 出典メモ | uspto-grants-2013_05 |