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Sulfuric Acid → N-(1-benzyl-3-methylpyrrolidin-3-yl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 1-Benzyl-3-methylpyrrolidin-3-OL | HCID 18629648 | — |
| 生成物 | N-(1-benzyl-3-methylpyrrolidin-3-yl)acetamide | HCID 13787481 | — |
反応手順
A solution of 1-benzyl-3-methylpyrrolidin-3-ol (5.94 g, 31.1 mmol) in MeCN (200 mL) was cooled in an ice bath and conc H2SO4 (25 mL) was added dropwise over 15 min. The ice bath was allowed to melt and the mixture was stirred at rt over the weekend. The mixture was poured onto crushed ice (600 mL). The mixture was evaporated under reduced pressure to remove MeCN. Solid K2CO3 was added in portions to the residue until it was basic. The mixture was extracted with CH2Cl2 (3×150 mL). The combined organic extracts were washed with brine (50 mL), dried over Na2SO4 and concentrated to leave N-(1-benzyl-3-methylpyrrolidin-3-yl)acetamide (4.01 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08828985B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b911826704eb433dac44479d5dc753f0 |
| 出典メモ | uspto-grants-2014_09 |