関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide | HCID 22467641 | — |
| 反応物 | HCID 178511715 | HCID 178511715 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 178522768 | HCID 178522768 | 84.2% |
反応手順
To a solution of 2-fluoro-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide (150 mg) in anhydrous pyridine (3 mL) was added trans-4-aminocyclohexanol (81.4 mg), and the mixture was stirred for 15 hours at ambient temperature, and then for 3 hours at 60° C. The mixture was partitioned between ethyl acetate and water. The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was subjected to a silica gel column chromatography eluting with a mixture of chloroform and methanol (20:1). The eluent was concentrated and the residue was triturated with diisopropyl ether to give 2-(trans-4-hydroxycyclohexylamino)-5-nitro-N-(1,3-benzodioxol-5-ylmethyl)benzamide as yellow powders (164 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06384080B1 |
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| 出典データセット | uspto-grants-2002_05 |
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| ORD ID | ord-51cea3d5a0df4652af0750f4f91785be |
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| 出典メモ | uspto-grants-2002_05 |
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