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4-(Pyrrolidin-1-yl)butan-1-amine → 4-Chloro-N-[4-(1-pyrrolidinyl)butyl]-2-pyridinecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-(Pyrrolidin-1-yl)butan-1-amine | HCID 2762762 | — |
| 反応物 | 4-chloropyridine-2-carbonyl Chloride | HCID 11095146 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-Chloro-N-[4-(1-pyrrolidinyl)butyl]-2-pyridinecarboxamide | HCID 85971931 | — |
反応手順
To a suspension of 4-chloro-pyridine-2-carbonyl chloride (8.88 g, 49 mmol) in THF (100 mL) was added at 0° C. 4-pyrrolidin-1-yl-butylamine (7.0 g, 49 mmol). The reaction was stirred for 18 h at RT. The mixture was diluted with EtOAc, washed several time with aqueous 6 N NaOH and then brine, dried over Na2SO4, filtered, and concentrated in vacuo. The crude material was purified by flash chromatography using a gradient CH2Cl2/MeOH/NH4OH (100%, 0%, 0% to 90%, 10%, 1%). The pure fractions were combined and the solvents removed under vacuum. The title compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07531553B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-62815154662f40f2b6291db7c0c97d64 |
| 出典メモ | uspto-grants-2009_05 |