Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Thiophene-3-carboxylic acid → 4-[3-(3-Thiophenecarbonylamino)propylthio]pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Thiophene-3-carboxylic acid | HCID 6918 | — |
| 반응물 | N-Hydroxysuccinimide | HCID 80170 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 4-(3-Aminopropylthio)pyridine | HCID 15227695 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-[3-(3-Thiophenecarbonylamino)propylthio]pyridine | HCID 19079093 | 76.1% |
반응 단계
To a solution of 1.00 g (7.80 mmol) of thiophene-3-carboxylic acid and 1.08 g (10.1 mmol) of N-hydroxysuccinimide in 70 ml of methylene chloride, 1.80 g (9.36 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 1 hour. Further, 1.31 g (7.80 mmol) of 4-(3-aminopropylthio)pyridine was added, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was washed with water and dried, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10) to obtain 1.65 g of the desired compound (yield: 76.1%, colorless powder).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05246948 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-98480977321a48fc9c80434e5c786ddb |
| 출처 메모 | uspto-grants-1993_09 |