참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 6-Bromoquipazine | HCID 130261 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | [(2R)-8-methyl-2,3-dihydro[1,4]dioxino[2,3-f]quinolin-2-yl]methyl4-bromobenzenesulfonate | HCID 20624762 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | HCID 44219922 | HCID 44219922 | 39.3% |
반응 단계
To a solution of [(2R)-8-methyl-2,3-dihydro[1,4]dioxino[2,3-f]quinolin-2-yl]methyl 4 bromobenzene sulfonate (2.31 g, 5.13 mmol) in dimethylsulfoxide (123 mL) is added the 6-bromo-2-piperazin-1-yl-quinoline of Step B (1.5 g, 5.13 mmol) and the mixture is heated at 75° C. under nitrogen overnight. The mixture is poured into saturated aqueous sodium bicarbonate and extracted with ethyl acetate. The extracts are dried over anhydrous magnesium sulfate and evaporated to dryness. The residue is flash chromatographed on silica gel Merck-60 using a gradient of methanol (0.5–2%) in ethyl acetate-hexane (55:45) to provide the title compound as an off-white solid (1.02 g), m.p. 153–154° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07153849B2 |
|---|
| 출처 데이터셋 | uspto-grants-2006_12 |
|---|
| ORD ID | ord-bb354057eb944558a4c9fedc147cdf05 |
|---|
| 출처 메모 | uspto-grants-2006_12 |
|---|