関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | N-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonoyl chloride | HCID 131733232 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N'-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonamide | HCID 117965458 | — |
反応手順
To a cold solution of N-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonoyl chloride (0.070 g, 0.267 mmol) in dry THF was added aq. ammonia. The reaction mass was stirred at 0-5° C. for 2-3 h. The reaction mass was quenched in water, neutralized with dilute acetic acid and extracted with DCM. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 0.040 g of the desired product. 1H NMR (300 MHz, DMSO d6): δ 6.29 (br s, 2H), 6.80 (d, J=8.4 Hz, 2H), 7.24 (d, J=9.3 Hz, 2H), 7.28-7.50 (m, 3H), 8.33 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09439890B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-e3b3e7e8935b47088e554424e5b52271 |
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| 出典メモ | uspto-grants-2016_09 |
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