Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Lithium Bromide → 4-(2-Bromoethyl)oxane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Lithium Bromide | HCID 82050 | — |
| 반응물 | 2-(Tetrahydro-2H-pyran-4-yl)ethyl methanesulfonate | HCID 22273083 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 4-(2-Bromoethyl)oxane | HCID 22637012 | 69.9% |
반응 단계
To 2-(tetrahydro-2H-pyran-4-yl)ethyl methanesulfonate (5.4 g) in dry acetone at room temperature was added lithium bromide (9 g) in one go. The reaction was heated to reflux for 4 hours, under nitrogen. The reaction was cooled to room temperature and concentrated in vacuo. The residue was taken up in dichloromethane (100 ml) and washed with water (50 ml). The organic layer was dried by passing through a hydrophobic frit, and concentrated in vacuo. The product was purified by silica chromatography (40 g) (ISCO) using a gradient elution of 0-50% cyclohexane:ethyl acetate to afford the title compound as a colourless oil (3.5 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07977344B2 |
| 출처 데이터셋 | uspto-grants-2011_07 |
| ORD ID | ord-886c78ff6a324304b1d02e82947b120c |
| 출처 메모 | uspto-grants-2011_07 |