Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Chloro-8-methoxy-2-methylquinoline → (rac)-1-(4-Chlorophenyl)-N*1*-(8-methoxy-2-methylquinolin-4-yl)-N*2*,N*2*-dimethylethane-1,2-diamine dihydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Chloro-8-methoxy-2-methylquinoline | HCID 807583 | — |
| 반응물 | (2-Amino-2-(4-chlorophenyl)ethyl)dimethylamine | HCID 16643575 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | (rac)-1-(4-Chlorophenyl)-N*1*-(8-methoxy-2-methylquinolin-4-yl)-N*2*,N*2*-dimethylethane-1,2-diamine dihydrochloride | HCID 131730511 | 60.4% |
반응 단계
4-Chloro-8-methoxy-2-methylquinoline (2.00 g, 9.63 mmole), 1-(4-chlorophenyl)N*2*,N*2*-dimethylethane-1,2-diamine (2.30 g, 11.6 mmole), sodium tert-butylate (1.3 g, 13.5 mmole), tris(dibenzylidenaceton)-dipalladium(0) (0.18 g, 0.193 mmole) and 2-dicyclohexyl-phosphino-2(N,N-dimethylamino)biphenyl (0.27 g, 0.674 mmole) were stirred at 150° C. under nitrogen atmosphere in a microwave oven for 30 min. The reaction mixture was dissolved in ethyl acetate and filtered. The filtrate was extracted with water. The organic phases were dried, concentrated and the residue was purified using silica gel chromatography, eluting with dichloromethane:methanol 90:10. Precipitation in isopropanol/HCl and in ethyl acetate gave the product (1.55 g, 36%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08420670B2 |
| 출처 데이터셋 | uspto-grants-2013_04 |
| ORD ID | ord-12c7456afd1f4763b019a5b648c41308 |
| 출처 메모 | uspto-grants-2013_04 |