関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Hydroxylamine HCl | HCID 21645 | — |
| 反応物 | Tert-butyl 4-cyanophenylcarbamate | HCID 10130644 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Tert-butyl 4-(N-hydroxycarbamimidoyl)-phenylcarbamate | HCID 53439229 | — |
反応手順
At RT, 1.40 g (20.16 mmol, 2.2 eq.) of hydroxylammonium chloride and 2.81 ml (20.16 mmol, 2.2 eq.) of triethylamine were added to a solution of 2.0 g (9.16 mmol) of tert-butyl-(4-cyanophenyl)carbamate in 45 ml of ethanol. The reaction mixture was heated under reflux for 4 h and concentrated under reduced pressure. The residue was stirred with 100 ml of water at RT for 1 h. The reaction mixture was filtered and the filter cake was washed with water. The residue was dissolved in ethyl acetate. The aqueous phase that remained was separated off and the organic phase was dried (sodium sulphate), filtered and concentrated under reduced pressure. The crude product was used for the next step without purification. Yield: 2.10 g (purity 95%, 87% of theory)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434690B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-2f4bc81327554caa957bda3a2531d281 |
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| 出典メモ | uspto-grants-2016_09 |
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