Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Iodide → N-[1-(3-methylbenzyl)-4-methyl-hexahydro-1H-1,4-diazepin-6-yl]-1-ethyl-1H-indazole-3-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | m-Xylyl chloride | HCID 12102 | — |
| 반응물 | N-(1-methylhexahydro-1H-1,4-diazepin-6-yl)-1-ethyl-1H-indazole-3-carboxamide | HCID 14999044 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | N-[1-(3-methylbenzyl)-4-methyl-hexahydro-1H-1,4-diazepin-6-yl]-1-ethyl-1H-indazole-3-carboxamide | HCID 14999045 | 78.4% |
반응 단계
A mixture of N-(1-methylhexahydro-1H-1,4-diazepin-6-yl)-1-ethyl-1H-indazole-3-carboxamide (1.8 g), potassium carbonate (4.1 g), sodium iodide (0.9 g), 3-methylbenzyl chloride (0.85 g) and methyl ethyl ketone (100 ml) is refluxed with stirring for 6 hours. After cooling, the reaction mixture is filtered, and the filtrate is concentrated under reduced pressure. The residue is chromatographed on silica gel with elution of chloroform-methanol (20:1). Fractions containing the title compound are pooled and evaporated under reduced pressure to give the title compound (1.9 g) as an oil. The free base thus obtained is converted to the fumarate of the title compound in a usual manner, m.p. 135°-137° C. (recrystallized from ethanol-diethyl ether).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05166341 |
| 출처 데이터셋 | uspto-grants-1992_11 |
| ORD ID | ord-eeb7f51a35804c3b9b3dbd092fa9d37a |
| 출처 메모 | uspto-grants-1992_11 |