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2,6-Lutidine → N-(cyanomethyl)-2-hydroxy-4-methoxy-N-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Lutidine | HCID 7937 | — |
| 反応物 | Acetonitrile, 2-(methylamino)- | HCID 36652 | — |
| 反応物 | 2-Hydroxy-4-methoxybenzoyl chloride | HCID 23118559 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(cyanomethyl)-2-hydroxy-4-methoxy-N-methylbenzamide | HCID 55207279 | — |
反応手順
To a solution of 2-hydroxy-4-methoxybenzoyl chloride (22.19 g, 118.9 mmol) in 500 CH2Cl2 were added (methylamino)acetonitrile (10 g, 142.7 mmol) and 2,6-lutidine (19.1 g, 178.4 mmol). The reaction was stirred at rt overnight. The reaction mixture was then partitioned between EtOAc and 1(N) aq HCl. Organic layer washed with 1(N) aq HCl (2×), dried over Na2SO4 and concentrated to light yellow viscous material (24.63 g, 94%). This material was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07691879B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-337927e2294b41c7ba3c1c1f19860c77 |
| 出典メモ | uspto-grants-2010_04 |