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1-Bromo-2-Chloroethane → 1-(2-Chloroethyl)-4-(methylsulfonyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Bromo-2-Chloroethane | HCID 7849 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(Methylsulfonyl)piperazine | HCID 709161 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(2-Chloroethyl)-4-(methylsulfonyl)piperazine | HCID 20158350 | — |
反応手順
A mixture of 1-(methylsulfonyl)piperazine (250 mg, 1.522 mmol), potassium carbonate (1262 mg, 9.13 mmol) and 1-bromo-2-chloroethane (1092 mg, 7.61 mmol) in acetonitrile (5 mL) was stirred for 6 hours at room temperature. LCMS indicated the formation of desired product. The reaction mixture was filtered to remove the white precipitate, then quenched with distilled water (10 mL), extracted with ethyl acetate (3×8 mL), the extracts were combined, dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the clean desired product as white solid (100 mg, 29%). LCMS: m/e 227.15 (M+H)+, 1.21 min (method 10).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846647B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-19ad2a3a85a444e3ba8bdb52476b5267 |
| 出典メモ | uspto-grants-2014_09 |