Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 3-Bromo-5-hydroxybenzenemethanol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3-Bromo-5-hydroxybenzoic acid | HCID 15735511 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-Bromo-5-hydroxybenzenemethanol | HCID 59496812 | 36% |
반응 단계
To a solution of 3-bromo-5-hydroxy-benzoic acid (5.0 g, 23.4 mmol) in 40 mL of THF was added a solution of 1M LiAlH4 (30 mL), and the resulting solution was heated to reflux for 2 h. After cooling to room temperature, the reaction mixture was poured on ice and acidified with 10% aq. HCl. The solution was then filtered under vacuum and the filtrate was extracted with EtOAc. The organic extract was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude material was purified by column chromatography (Isco™ 120 g) using 50% ethyl acetate/hexanes as eluting solvents to afford the title compound as a white solid (1.7 g, 36% yield). HR-ES(−) calcd for C7H7O2Br [M−H]− 200.9556, observed 200.9557.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08088936B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-0d08bb7fd2b14521a2d4adaec785907c |
| 출처 메모 | uspto-grants-2012_01 |