Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylsilane → 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylsilane | HCID 12052 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran-4-one | HCID 14755364 | — |
| 용매 | Trifluoroacetic acid | HCID 6422 | — |
| 생성물 | 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran | HCID 15840550 | 150.5% |
반응 단계
TO a solution of 6-bromo-2,2-dimethyl-2,3-dihydro-4H-1-benzopyran-4-one (7.57 g) in trifluoroacetic acid (21.4 ml) was added at room temperature triethylsilane (10.4 ml), and the mixture was stirred for 4 days. To the mixture was added triethylsilane (7.1 ml), and the mixture was stirred at 50° C. for 24 hours. To the mixture was added at 0° C. 12N sodium hydroxide solution to make the solution alkaline, and the mixture was extracted with diethylether. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure. The residue was purified with silica gel column chromatography (hexane) to give colorless oil of 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran (10.77 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06235771B1 |
| 출처 데이터셋 | uspto-grants-2001_05 |
| ORD ID | ord-f720480f9e6b4f629a9321a3a5635523 |
| 출처 메모 | uspto-grants-2001_05 |