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Hydrochloric Acid → 2,5 Dichlorobenzaldehyde-chloro-oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | Benzaldehyde, 2,6-dichloro-, oxime | HCID 91328 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,5 Dichlorobenzaldehyde-chloro-oxime | HCID 86642481 | — |
反応手順
2,6-Dichloro-benzaldehyde oxime (7.6 g, 40 mmol) is dissolved in 56 mL of DMF and N-chlorosuccinimide (5.9 g, 44.0 mmol) is added followed by a catalytic amount of HCl gas. The reaction mixture is stirred overnight. The reaction mixture is partitioned between ether and water. The layers are separated and the ether layer is washed with brine and is dried over sodium sulfate. The ether layer is filtered and the solvent is removed under reduced pressure to yield the crude product. The crude product is purified via chromatography using a gradient of 10% ethyl acetate in hexanes to 15% ethyl acetate in hexanes to yield the title compound. 1H-NMR (400 MHz, CDCl3) δ 8.76 (broad, 1H), 7.38-7.26 (m, 3H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08153624B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-4e199cffcfd24866a61c24e7a6bf75cf |
| 出典メモ | uspto-grants-2012_04 |