Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Methylimidazole → 1-O-(p-toluenesulfonyl)-2-methylene-1,3-propanediol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Methylimidazole | HCID 1390 | — |
| 반응물 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 반응물 | Dibutyltin oxide | HCID 61221 | — |
| 반응물 | 1,3-Propanediol, 2-methylene- | HCID 77048 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-O-(p-toluenesulfonyl)-2-methylene-1,3-propanediol | HCID 18475464 | 32.4% |
반응 단계
2-Methylene-1,3-propanediol (480 mg) and dibutyltinoxide (1,7 g) were dissolved in toluene (30 ml) and the resulting suspension was refluxed for 1 hour eliminating water with the help of a Dean-Stark apparatus. The flask was cooled down to room temperature and then, N-methyl-imidazol (797 ml) and tosyl chloride (1,56 g) were added. After 15 minutes stirring, the reaction crude was directly purified by column chromatography (hexane-ethyl acetate v/v from 7:1 to 1:1). The title compound (428 mg) was obtained as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06410528B1 |
| 출처 데이터셋 | uspto-grants-2002_06 |
| ORD ID | ord-79d8c75fdd72464a9b13680a82011c96 |
| 출처 메모 | uspto-grants-2002_06 |