関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydroxylamine HCl | HCID 21645 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 4-(4-t-Butylcyclohexyl)-3-(4-butylpiperazin-1-yl)benzaldehyde | HCID 23142500 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(4-t-Butylcyclohexyl)-3-(4-butylpiperazin-1-yl)benzaldehydeoxime | HCID 74020552 | 105.6% |
反応手順
To a mixture of the crude product of 4-(4-t-butylcyclohexyl)-3-(4-butylpiperazin-1-yl)benzaldehyde produced in Example (101b) (247 mg), hydroxylammonium chloride (134 mg, 1.93 mmol) and ethanol (10 mL) were added sodium acetate (193 mg, 2.35 mmol) and water (1.5 mL), followed by stirring for 2 hours at room temperature. The reaction mixture was poured into ice water, and then ethyl acetate and saturated aqueous solution of ammonium chloride were added and extraction was performed with ethyl acetate. The separated organic layer was washed with brine and then dried over anhydrous sodium sulfate. The desiccant was filtered off, and the filtrate was concentrated under reduced pressure to give 271 mg of a crude product of the title compound as a light yellow solid. This product was directly used without purification for the following reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425554B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-ec9889d94e2147858c604e0aa01348c5 |
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| 出典メモ | uspto-grants-2008_09 |
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