Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 4-(3-(N-(2-thienylmethyl)amino)propylthio]pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | (2-Thienylmethyl)amine | HCID 34005 | — |
| 반응물 | 4-(3-Hydroxypropylthio)pyridine | HCID 19079134 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(3-(N-(2-thienylmethyl)amino)propylthio]pyridine | HCID 19079184 | 29.1% |
반응 단계
In 200 ml of methylene chloride were dissolved 10.34 g (61.1 mmol) of 4-(3-hydroxypropylthio)pyridine and 10.2 ml (73.3 mmol) of triethylamine, methanesulfonyl chloride [5.7 ml (73.3 mmol)] was added, and 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. Then the solvent was distilled off. To 8.05 g of the residue was added 3.3 ml (32.5 mmol) of 2-thiophenemethylamine. The mixture was heated at 80° C. for 3 hours. After cooling, the mixture was purified by column chromatography (eluent: chloroform/methanol=25:1) to obtain 2.5 g of the desired compound (yield: 29.1%, yellow oil).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05246948 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-80d6d35a6b1b4822a93a6f325c74f83a |
| 출처 메모 | uspto-grants-1993_09 |