Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 4-(4-Fluorobenzoyl)-1-(2-hydroxyethyl)piperidine | HCID 14892165 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride | HCID 67575338 | 96.3% |
반응 단계
In an atmosphere of dry air, 4-(4-fluorobenzoyl)-1-(2-hydroxyethyl)piperidine (1.96 g, 7.8 mmol) was dissolved in methylene chloride (10 ml) to which, with cooling in an ice bath, were subsequently added dropwise DMF (0.1 ml) and thionyl chloride (2.5 ml, 34.2 mmol). After 7 hours of stirring at room temperature, the solvent was removed by evaporation, and the resulting residue was subjected to azeotropic distillation using benzene (15 ml×2). Thereafter, the thus obtained residue was washed with an ether-methylene chloride (4:1) mixture solution (30 ml) to obtain 2.3 g (96.3%) of the title compound in the form of light beige powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05728835 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-761b0c03342a44cd91f901367699772b |
| 출처 메모 | uspto-grants-1998_03 |