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 | Ethyl 6-chloro-4-(cyclobutylamino)nicotinate | HCID 89689654 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Chloro-4-(isopropylamino)nicotinohydrazide | HCID 89689668 | — |
反応手順
To a stirred solution of ethyl 6-chloro-4-(isopropylamino)nicotinate (2) (3 g, 12.39 mmol) in ethanol (10 mL), hydrazine hydrate (3 mL) was added and refluxed at 80° C. for 3 h. The reaction mixture was cooled and concentrated to obtain crude compound. The residue obtained was triturated with diethyl ether and hexane and filtered to get solid, 6-chloro-4-(isopropylamino)nicotinohydrazide (10). LC/MS: Acquity BEH C18 2.1×50 mm, 1.8 micron; Solvent A=0.1% TFA in water; Solvent B=0.1% TFA in ACN; gradient 0-100% B over 2 min; retention time: 0.58 min; LCMS (ES-API), m/z 229.6 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09242976B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-d80d4f3e2ef447cd9a5fda1d07c38468 |
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| 出典メモ | uspto-grants-2016_01 |
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