Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-(Methylthio)-1-propanol → 2-Bromo-1,3-dimethyl-5-[3-(methylthio)propoxy]benzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-(Methylthio)-1-propanol | HCID 10448 | — |
| 반응물 | Tributylphosphine | HCID 13831 | — |
| 반응물 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 반응물 | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 2-Bromo-1,3-dimethyl-5-[3-(methylthio)propoxy]benzene | HCID 59342575 | 87% |
반응 단계
To a solution of 4-bromo-3,5-dimethylphenol (4.02 g, 20.0 mmol), 3-(methylthio)-1-propanol (2.12 g, 20.0 mmol) and tributylphosphine (7.97 mL, 32.0 mmol) in toluene (320 mL) was added 1,1′-(azodicarbonyl)dipiperidine (8.07 g, 32.0 mmol), and the mixture was stirred at room temperature for 18 hr under nitrogen atmosphere. Hexane (160 mL) was added to the reaction mixture, the insoluble substance was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=0:100-25:75) to give the title compound (5.03 g, yield 87%) as a pale-yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08598226B2 |
| 출처 데이터셋 | uspto-grants-2013_12 |
| ORD ID | ord-e340654a9ac04344b2995fe6418edb08 |
| 출처 메모 | uspto-grants-2013_12 |