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 | tert-Butyl 2-nitro-4-(thiophen-2-yl)phenylcarbamate | HCID 59736984 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | tert-Butyl (2-amino-4-(thiophen-2-yl)phenyl)carbamate | HCID 57717474 | 83% |
反応手順
To a solution of tert-butyl (2-nitro-4-(thiophen-2-yl)phenyl)carbamate (1.6 g, 4.99 mmol, 1 eq.) in methanol (20 mL) was added hydrazine hydrate (14 mL) and ferric chloride (0.05 g, 0.3 mmol, 0.06 eq.). The resulting mixture was warmed to 60° C. and stirred for 2 h. The reaction was then filtered through Celite, the solids were washed with MeOH. The filtrate was concentrated under reduced pressure. Water was added to the residue and the suspension was stirred for 1 h. The obtained solid was filtered, washed with hexanes then dried to yield tert-butyl (2-amino-4-(thiophen-2-yl)phenyl)carbamate (1.2 g, 83% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09447030B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-b1815fdfd6c64e5a97cd19b00096e39b |
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| 出典メモ | uspto-grants-2016_09 |
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