Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-8-(2-acetylethyl)-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Buten-2-ol | HCID 11716 | — |
| 반응물 | 2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-8-iodo-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine | HCID 23359151 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-8-(2-acetylethyl)-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine | HCID 23359148 | 61.3% |
반응 단계
0.2 g of (±)-3-buten-2-ol, 1.4 mg of palladium (II) acetate and 0.27 g of triethylamine were added to 1.36 g of 2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-8-iodo-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine obtain in Reference example 73 dissolved in 2.5 ml of acetonitrile and the mixture was refluxed under heating for 5.5 hours. After 60 ml of methylene chloride and 60 ml of ice water were added to this reaction mixture, the organic layer was separated, washed with water and dried over anhydrous sodium sulfate. After the solvent was removed, the residue was applied to silica gel column chromatography to obtain 0.76 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05591752 |
| 출처 데이터셋 | uspto-grants-1997_01 |
| ORD ID | ord-dea302f230154be58f444459c1e69e67 |
| 출처 메모 | uspto-grants-1997_01 |