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 | 2,4-Dichloro-6-phenylpyrimidine | HCID 241554 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 20805788 | HCID 20805788 | — |
反応手順
To a solution of 2,4-dichloro-6-phenylpyrimidine (224 mg, 1 mmol) in 1 mL of 1,4-dioxane was added 300 uL of hydrazine hydrate. Stirring was continued at room temperature and the reaction monitored by thin layer chromatography (30% ethyl acetate/hexanes). When the starting material was consumed, 2 mL of water was added and the resultant precipitate was collected on a filter to afford 2-chloro-4-hydrazinyl-6-phenylpyrimidine as a yellow solid. The damp solid was suspended in 2 mL of ethanol, to which was added 220 mg of 4-trifluoromethoxybenzaldehyde. Within 5 minutes the solution became clear and then reprecipitated material. The product, 2-chloro-4-phenyl-6-(2-(4-(trifluoromethoxy)benzylidene)hydrazinyl)pyrimidine (XX), was collected by filtration and dried to afford 150 mg of a solid. ESI/MS 392.973, 395.002 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09321735B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-d54cb5e4acd243dd83d68ec7933d6462 |
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| 出典メモ | uspto-grants-2016_04 |
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