関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Diethyl Sulfate | HCID 6163 | — |
| 反応物 | Benzenamine, 2-(2-methoxyethoxy)-5-nitro- | HCID 114242 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Ethylamino-4-nitro-beta-methoxyethoxybenzene | HCID 20235291 | 89.5% |
反応手順
185 g of diethyl sulfate (1.2 mole) are added dropwise to a mixture of 577 g of toluene and 212 g of 2-amino-4-nitro-β-methoxyethoxybenzene (1 mole). The mixture is stirred at 80° C. for 5 hours and then neutralized with 169 g of 14% strength aqueous ammonia. The toluene is removed by azeotropic distillation and the aqueous residue is adjusted to pH 0.4 with 165 g of concentrated hydrochloric acid. 10 g of keiselguhr and 0.5 g of zinc dust are added to the mixture. It is then boiled under reflux for 30 minutes and finally filtered hot. The filtrate is adjusted to pH 2 with 120 ml of concentrated sodium hydroxide solution. The precipitate is filtered off with suction and dried in vacuo. 215 g of 2-ethylamino-4-nitro-β-methoxyethoxybenzene are obtained, which corresponds to a yield of 76% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04612396 |
|---|
| 出典データセット | uspto-grants-1986_09 |
|---|
| ORD ID | ord-e5ff9b6f0fc54b39a4dbf4e30b2fab26 |
|---|
| 出典メモ | uspto-grants-1986_09 |
|---|