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Hydrazine hydrate (1:1) → 4-Amino-N-(1-(5-aminopentyl)piperidin-4-ylmethyl)-5-chloro-2-methoxybenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 4-amino-5-chloro-N-(1-(5-(2,3-dihydro-1,3-dioxo-1H-isoindol-2-yl)pentyl)piperidin-4-ylmethyl)-2-methoxybenzamide | HCID 54379569 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Amino-N-(1-(5-aminopentyl)piperidin-4-ylmethyl)-5-chloro-2-methoxybenzamide | HCID 54008363 | 82.6% |
反応手順
Hydrazine monohydrate (11.3 ml) was added to a solution of 4-amino-5-chloro-N-(1-(5-(2,3-dihydro-1,3-dioxo-1 H-isoindol-2-yl)pentyl)-piperidin-4-ylmethyl)-2-methoxybenzamide (60 g) in ethanol (0.6 L), and the mixture was refluxed under heating for 4 hr. The precipitated crystals were filtered off, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform:methanol=10:1) to give 37.0 g of 4-amino-N-(1-(5-aminopentyl)piperidin-4-ylmethyl) -5-chloro-2-methoxybenzamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05864039 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-e93f889a6b074315999bb4143df17942 |
| 出典メモ | uspto-grants-1999_01 |