Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonium Chloride → 1-[1-(4-Fluorophenethyl)piperidin-4-yl]-6-acetylindoline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Dimethylacetamide | HCID 31374 | — |
| 반응물 | 1-[1-(4-Fluorophenethyl)piperidin-4-yl]-6-bromoindoline | HCID 22037889 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-[1-(4-Fluorophenethyl)piperidin-4-yl]-6-acetylindoline | HCID 22038117 | 27% |
반응 단계
A 2.5 M solution (1.5 ml) of n-butyllithium in hexane was added dropwise at −78° C. into a solution (30 ml) of 1-[1-(4-fluorophenethyl)piperidin-4-yl]-6-bromoindoline (1.0 g) in tetrahydrofuran over 5 min. After 10 min, dimethylacetamide (0.34 ml) was added thereto and the resultant mixture was warmed to room temperature. Next, a saturated aqueous solution of ammonium chloride and ethyl acetate were added thereto to and the layers were separated. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by NH-silica gel column chromatography (hexane/ethyl acetate system) to give the title compound (250 mg) as a yellow powder (yield: 27%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07071201B2 |
| 출처 데이터셋 | uspto-grants-2006_07 |
| ORD ID | ord-e3eec821340f44e9a277867fc7a6326b |
| 출처 메모 | uspto-grants-2006_07 |