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Veratroyl chloride → N-[2-chloro-5-(3-dimethylaminobenzamido)4-fluorophenyl]-3,4-dimethoxybenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Veratroyl chloride | HCID 77070 | — |
| 反応物 | N-(5-amino-4-chloro-2-fluorophenyl)-3-dimethylaminobenzamide | HCID 22732310 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-[2-chloro-5-(3-dimethylaminobenzamido)4-fluorophenyl]-3,4-dimethoxybenzamide | HCID 9847600 | 27.9% |
反応手順
A mixture of 3,4-dimethoxybenzoyl chloride (0.5 g), N-(5-amino-4-chloro-2-fluorophenyl)-3-dimethylaminobenzamide (0.781 g) and pyridine (8 ml) was stirred at ambient temperature for 18 hours. The mixture was evaporated and the residue was partitioned between methylene chloride and a saturated aqueous copper sulphate solution. The organic phase was washed in turn with water and a saturated aqueous sodium chloride solution, dried (MgSO4) and evaporated. The residue was purified by column chromatography on silica using a 99:1 mixture of methylene chloride and methanol as eluent. There was thus obtained the title compound as a solid (0.328 g);
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06465455B1 |
| 出典データセット | uspto-grants-2002_10 |
| ORD ID | ord-206ad1cdf15246a18208d54689358a07 |
| 出典メモ | uspto-grants-2002_10 |