化工社化工社 化学情報印刷レポート · 研究参考用
Phosphorus oxychloride → 3-{[4-Chloro-5-fluoro-2-(methoxymethoxy)benzoyl]amino}thiophene-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3-Aminothiophene-2-carboxamide | HCID 518993 | — |
| 反応物 | Lithium 4-chloro-5-fluoro-2-(methoxymethoxy)benzoate | HCID 69077744 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3-{[4-Chloro-5-fluoro-2-(methoxymethoxy)benzoyl]amino}thiophene-2-carboxamide | HCID 69074647 | — |
反応手順
n-butyllithium was added to a diethyl ether solution of 1-bromo-4-chloro-5-fluoro-2-(methoxymethoxy)benzene in a dry ice-acetone bath and stirred for one hour. The reaction solution was added to a mixture of dry ice and diethyl ether and stirred for two hours to give lithium 4-chloro-5-fluoro-2-(methoxymethoxy)benzoate. Phosphorus oxychloride was added to a mixture of the obtained lithium 4-chloro-5-fluoro-2-(methoxymethoxy)benzoate, 3-aminothiophene-2-carboxamide and pyridine in a MeOH ice bath and stirred for one hour to give 3-{[4-chloro-5-fluoro-2-(methoxymethoxy)benzoyl]amino}thiophene-2-carboxamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07557112B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-b6f1d9a9f6e644cfa86965f3b6902012 |
| 出典メモ | uspto-grants-2009_07 |