Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Chloroaniline → 4'-Chloro-3-hydroxy-2-nitrobenzanilide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Chloroaniline | HCID 7812 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 3-Hydroxy-2-nitrobenzoic acid | HCID 293291 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4'-Chloro-3-hydroxy-2-nitrobenzanilide | HCID 17856979 | 92.9% |
반응 단계
3-Hydroxy-2-nitrobenzoic acid (2.00 g) was dissolved in 110 ml of N,N-dimethylformamide, then 1.53 g of 4-chloroaniline, 3.15 g of 1-ethyl-3-[3-(N,N-dimethylamino) propyl]carbodiimide hydrochloride and 2.21 g of 1-hydroxybenzotriazole were added thereto and the mixture was stirred at room temperature for 4 days. The reaction solution was concentrated in vacuo, a saturated saline was added to the concentrate and the mixture was extracted with chloroform. The organic layer was dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by means of a silica gel column chromatography using chloroform:methanol (100:1) as an eluate to give 2.97 g of 4′-chloro-3-hydroxy-2-nitrobenzanilide.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07504417B2 |
| 출처 데이터셋 | uspto-grants-2009_03 |
| ORD ID | ord-4cfcc01f8e9d4cd8be424b588c6114d4 |
| 출처 메모 | uspto-grants-2009_03 |