참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Diethyl Sulfate | HCID 6163 | — |
| 반응물 | Benzenamine, 2-(2-methoxyethoxy)-5-nitro- | HCID 114242 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 2-Ethylamino-4-nitro-beta-methoxyethoxybenzene | HCID 20235291 | 89.5% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04612396 |
|---|
| 출처 데이터셋 | uspto-grants-1986_09 |
|---|
| ORD ID | ord-e5ff9b6f0fc54b39a4dbf4e30b2fab26 |
|---|
| 출처 메모 | uspto-grants-1986_09 |
|---|