Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethanol → Benzoic acid, 4-chloro-2-hydroxy-, ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 4-Chlorosalicylic acid | HCID 78782 | — |
| 반응물 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 반응물 | Dimethylaminopropyl carbodiimide hydrochloride | HCID 21899179 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Benzoic acid, 4-chloro-2-hydroxy-, ethyl ester | HCID 12548597 | 43.5% |
반응 단계
4-Chlorosalicylic acid (344 mg), 1-ethyl-3-(3-dimethylaminopropylcarbodiimide hydrochloride (420 mg), 1-hydroxybenzotriazole hydrate (337 mg), and ethanol (2 ml) were dissolved in N,N-dimethylformamide to prepare a solution which was then stirred at room temperature overnight. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography using acetone-hexane to give ethyl 4-chlorosalicylate (174 mg, yield 43%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07560558B2 |
| 출처 데이터셋 | uspto-grants-2009_07 |
| ORD ID | ord-63f94f5e381e42159b80935652026ca1 |
| 출처 메모 | uspto-grants-2009_07 |