関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-amino-5-chloro-N-(4-chlorophenyl)benzamide | HCID 4186019 | — |
| 反応物 | 3-Chloro-4-chloromethyl-2-(chlorocarbonyl)thiophene | HCID 18376676 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 18376557 | HCID 18376557 | 80% |
反応手順
To a solution of 3-chloro-4-chloromethyl-2-(chlorocarbonyl)thiophene (3.1 g, 13.5 mmol) in methylene chloride (40 mL) at 0° C. was added N-(4-chlorophenyl)-2-amino-5-chlorobenzamide (3.8 g, 13.5 mmol), followed after 5 minutes by pyridine (1.6 mL, 16 mmol). The mixture was warmed to ambient temperature. After 17 hours, the mixture was concentrated of all volatiles in vacuo. The resulting solid was triturated with water and a small amount of acetonitrile and dried in vacuo to afford 5.1 g (80% yield) of N-(4-chlorophenyl)-2-[((4-(chloromethyl)-3-chlorothiophen-2-yl)carbonyl)amino]-5-chlorobenzamide as a tan powder: NMR (DMSO-d6) 11.1 (s, 1), 10.8 (s, 1), 8.3 (d, 1), 8.2 (s, 1), 7.9 (s, 1), 7.7 (d, 2), 7.6 (dd, 1), 7.4 (d, 2), 4.8 (s, 2) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06140351 |
|---|
| 出典データセット | uspto-grants-2000_10 |
|---|
| ORD ID | ord-59e6d36c5cf741ff976e42886025cd67 |
|---|
| 出典メモ | uspto-grants-2000_10 |
|---|