関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | 4-Bromo-2,5-difluorobenzoic acid | HCID 822857 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 4-Bromo-5-fluoro-2-hydrazinylbenzoic acid hydrochloride | HCID 76848196 | 44% |
反応手順
A mixture of 4-bromo-2,5-difluorobenzoic acid (2.50 g, 10.6 mmol) and hydrazine (3.81 mL, 121 mmol) in N-methyl-2-pyrrolidinone (2 mL) was heated at 95° C. for 4 h. The cooled mixture was poured into vigorously stirred 6 M aqueous HCl (400 mL) which was cooled in an NaCl-ice bath. The resulting precipitate was collected by filtration, washed with 6 M aqueous HCl (200 mL) and dried under vacuum to give 4-bromo-5-fluoro-2-hydrazinylbenzoic acid hydrochloride as a yellow solid (1.88 g, 71% purity, 44% yield), used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09334290B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-7d586237e60148f69ccfc0d9b881c500 |
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| 出典メモ | uspto-grants-2016_05 |
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