関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ethanesulfonamide | HCID 73702 | — |
| 反応物 | 2-Chloro-3-nitro-5-(trifluoromethyl)pyridine | HCID 4736950 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide | HCID 10851681 | 54.5% |
反応手順
3.1 g of ethanesulfonamide was dissolved in 50 ml of dry tetrahydrofuran, and 1.2 g of 60% sodium hydride was added thereto under cooling with ice. After completion of the addition, the mixture was reacted for one hour under reflux. After cooling, 5.0 g of 2-chloro-3-nitro-5-trifluoromethylpyridine was added thereto, and then the mixture was reacted for 7 hours under reflux. After completion of the reaction, the reaction product was poured into 200 ml of water. Undissolved materials in water were extracted with ethyl ether and removed. Then, the aqueous layer was weakly acidified with dilute hydrochloric acid. Precipitated crystals were collected by filtration and dried to obtain 3.6 g of N-(3-nitro-5-trifluoromethyl-2-pyridyl)ethanesulfonamide having a melting point of from 160° to 163° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05260320 |
|---|
| 出典データセット | uspto-grants-1993_11 |
|---|
| ORD ID | ord-da25dd324d444ea195b905ca178bf557 |
|---|
| 出典メモ | uspto-grants-1993_11 |
|---|