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Pyridine → 4-Chloro-N-methoxy-N-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Chlorobenzoyl chloride | HCID 8501 | — |
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Chloro-N-methoxy-N-methylbenzamide | HCID 11275663 | — |
反応手順
Pyridine (27.6 mL, 343 mmol) was added to N,O-dimethylhydroxylamine hydrochloride (16.7 g, 172 mmol) in DCM (400 mL). 4-Chlorobenzoyl chloride (20 mL, 156 mmol) was then added and the mixture was stirred at room temperature for 3 days. Solids were removed by vacuum filtration and washed with DCM. The filtrate was washed with 1 N aqueous HCl followed by water. The organic phase was dried (Na2SO4), filtered, and concentrated, affording the crude title compound as a colorless liquid which was used without purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09328095B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-7bf08be3d416434dba3d9cd6cc37e776 |
| 出典メモ | uspto-grants-2016_05 |