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Pyrrolidine → 1-(5-Chloro-2-nitrobenzyl)pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 5-Chloro-2-nitrobenzaldehyde | HCID 81123 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(5-Chloro-2-nitrobenzyl)pyrrolidine | HCID 783395 | — |
反応手順
Pyrrolidine (4 mL, 48.5 mmol) was added to a solution of 5-chloro-2-nitrobenzaldehyde (6 g, 32.2 mmol) in dichloromethane (150 mL) and the solution was stirred at room temperature for 30 minutes. The solution was then cooled in ice, and sodium triacetoxyborohydride (10.3 g, 48.5 mmol) was added portionwise. Once addition was complete, the reaction was stirred at room temperature for 4 hours. The reaction was washed with sodium carbonate solution, dried over MgSO4 and evaporated under reduced pressure. The residual oil was purified by column chromatography on silica gel using ethyl acetate:pentane (86:14) to afford the title compound as a pale yellow solid, 6.3 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745630B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-316009a3be204a12ba994ecef51047aa |
| 出典メモ | uspto-grants-2010_06 |