Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,6-Dimethylmorpholine → 6-Chloro-1-cyclopropyl-7-(2,6-dimethylmorpholin-4-yl)-8-fluoro-4-oxo-quinoline-3-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,6-Dimethylmorpholine | HCID 110862 | — |
| 반응물 | Diazabicyclo(2.2.2)octane | HCID 136165 | — |
| 반응물 | 6-Chloro-1-cyclopropyl-7,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid | HCID 13579163 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 6-Chloro-1-cyclopropyl-7-(2,6-dimethylmorpholin-4-yl)-8-fluoro-4-oxo-quinoline-3-carboxylic acid | HCID 483106 | 41% |
반응 단계
3 g (10 mmol) of the product from Example A in 35 ml of dimethyl sulphoxide are heated at 140° with 1.2 g (10 mmol) of 2,6-dimethylmorpholine and 2.2 g (20 mmol) of diazabicyclo[2.2.2]octane for 5 hours. The mixture is concentrated under high vacuum, stirred with 30 ml of water, the pH is adjusted to 6 with 2N hydrochloric acid, and the precipitate is filtered off with suction and recrystallized from glycol monomethyl ether. 1.6 g (41% of theory) of 6-chloro-1-cyclopropyl-8-fluoro-1,4-dihydro-7-(2,6-dimethyl-4-morpholinyl)-4-oxo-3-quinolinecarboxylic acid of melting point 258°-261° (with decomposition) is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05468861 |
| 출처 데이터셋 | uspto-grants-1995_11 |
| ORD ID | ord-422f5174584a4930ae1d2a19049950f0 |
| 출처 메모 | uspto-grants-1995_11 |