Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitrogen mustard hydrochloride → 3-Bromo-8-(4-methyl-piperazin-1-yl)-quinoline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitrogen mustard hydrochloride | HCID 5935 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 3-Bromoquinolin-8-amine | HCID 15112545 | — |
| 용매 | 1-Butanol | HCID 263 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Bromo-8-(4-methyl-piperazin-1-yl)-quinoline | HCID 67313624 | 49% |
반응 단계
bis-(2-Chloro-ethyl)-methyl-amine hydrochloride (3.7 g, 19.2 mmol) and sodium carbonate (9.0 g, 85 mmol) were added to a suspension of 3-bromo-quinolin-8-ylamine (3.9 g, 17.5 mmol) (for synthesis see Gershon et al., Monatsh. Chem., 1991, 122, 935) in n-butanol (70 ml). The stirred suspension was heated at reflux for 72 h. The reaction mixture was cooled to ambient temperature, diluted with dichloromethane (300 ml) and the solution washed with water (300 ml), dried (MgSO4) and concentrated in vacuo to an oil. The oil was purified by chromatography over silica gel eluting with a gradient of methanol/dichloromethane to afford the title compound (D1) as an oil (2.6 g, 8.5 mmol, 49%);
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07977337B2 |
| 출처 데이터셋 | uspto-grants-2011_07 |
| ORD ID | ord-e91a874730e34600a644101cce5a62a8 |
| 출처 메모 | uspto-grants-2011_07 |