Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 9-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Trimethylsilyl iodide | HCID 85247 | — |
| 반응물 | 3-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester | HCID 9951561 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 9-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide | HCID 21963712 | 97% |
반응 단계
Add iodotrimethylsilane (1.87 mL, 13.16 mmol) to a solution of 3-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester (2.06 g, 5.48 mmol) in dichloromethane (40 mL). Stir the solution at room temperature under nitrogen overnight. Add methanol (3.2 mL, 78.93 mmol) dropwise, and stir the reaction at room temperature for 30 minutes. Concentrate the reaction, add to diethyl ether, sonicate, and filtere. Dry the solids on a vacuum pump to give 2.36 g of the title compound as a tan solid, 97% yield. 1H NMR: consistent with structure. MS (ion spray) 318 (M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07101891B2 |
| 출처 데이터셋 | uspto-grants-2006_09 |
| ORD ID | ord-769fcdf1cdd8433c89c93ffe0bcf8a88 |
| 출처 메모 | uspto-grants-2006_09 |