Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Boron tribromide → 4-Cyano-4-(3-hydroxyphenyl)-3,4,5,6-tetrahydro-2H-pyran
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Boron tribromide | HCID 25134 | — |
| 반응물 | 4-(3-Methoxyphenyl)oxane-4-carbonitrile | HCID 18786366 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Cyano-4-(3-hydroxyphenyl)-3,4,5,6-tetrahydro-2H-pyran | HCID 11287160 | 68% |
반응 단계
To a dichloromethane (80 ml) solution of 4-cyano-4-(3-methoxyphenyl)-3,4,5,6-tetrahydro-2H-pyran (2.32 g, 10.35 mmol) cooled to 0° C. was added boron tribromide (3.15 ml, 33.3 mmol) dropwise over 10 min. The ice-bath was removed and the reaction mixture stirred at ambient temperature for 19 h, and then at reflux for 4 h. The reaction mixture was cooled and poured into water (150 ml). The organic layer was separated and the aqueous layer was extracted with ethyl acetate (50 ml×3). The combined organic extracts were washed with brine (50 ml), dried (MgSO4) and concentrated in vacuo. The crude product was crystallized from isopropyl ether to afford titled compound as off-white solids (1.43 g, 66%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05883106 |
| 출처 데이터셋 | uspto-grants-1999_03 |
| ORD ID | ord-1971f387252f422bb3176677c9bfffff |
| 출처 메모 | uspto-grants-1999_03 |