Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 4-[3-(2-Thenoylamino)propylthio]pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Thiophenecarbonyl chloride | HCID 78928 | — |
| 반응물 | 4-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079259 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-[3-(2-Thenoylamino)propylthio]pyridine | HCID 15231491 | 70.5% |
반응 단계
To a solution of 10.0 g (41.5 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 27.7 ml (200 mmol) of triethylamine in 100 ml of methylene chloride, 5.35 ml (50.0 mmol) of 2-thenoyl chloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water and dried, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:20) to obtain powder. The powder was recrystallized from methanol/ethyl acetate (=1:20) to obtain 8.05 g of the desired compound (yield: 70.5%, yellow prisms).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05246948 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-11093efb280540518b66f99ed8c2be55 |
| 출처 메모 | uspto-grants-1993_09 |