Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus tribromide → 3,4-Methylenedioxyphenethyl bromide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus tribromide | HCID 24614 | — |
| 반응물 | 2-(1,3-Dioxaindan-5-yl)ethan-1-ol | HCID 2759846 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 생성물 | 3,4-Methylenedioxyphenethyl bromide | HCID 12207224 | 121.1% |
반응 단계
A solution of phosphorus tribromide (8.1 g) in carbon tetrachloride (50 ml) was added dropwise over 30 minutes to a stirred solution of 3,4-methylenedioxyphenethyl alcohol (15.0 g) (see Preparation 5) in carbon tetrachloride (200 ml) and the mixture was heated under reflux for 3 hours, washed sequentially with water (twice), 5M aqueous sodium hydroxide solution and water, dried over magnesium sulphate and evaporated. The residue was purified by chromatography on silica (100 g) using carbon tetrachloride as the eluant. Appropriate fractions were combined and evaporated to give the title compound as a pale yellow oil (8.3 g, 40%), which was characterised by its 1H-NMR spectrum.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05486527 |
| 출처 데이터셋 | uspto-grants-1996_01 |
| ORD ID | ord-d8498382db174ecc82a5bba16c88d659 |
| 출처 메모 | uspto-grants-1996_01 |