참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cyanide | HCID 5975 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | HCID 178418689 | HCID 178418689 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 1,1'-Bipiperidine | HCID 68279 | 79% |
반응 단계
The cyanide (4.87 g, 15 mmol) was taken up in THF (75 ml). CH3MgBr (25 ml of a 3.0 M solution in Et2O) was added to the reaction mixture at 0° C. The solution was allowed to warm to 25° C. and was stirred at that temperature for 18 h. The solution was partitioned between 25 wt % aqueous solution of sodium citrate and EtOAc. The aqueous layer was extracted with EtOAc. The combined EtOAc layers were washed with brine and dried (Na2SO4). Filtration and concentration gave a yellow oil. Purification via flash chromatography (95/5 to 90/10 EtOAc/MeOH. SiO2) gave 3.7 g (79%) of the piperidino-piperidine 12 as a yellow gum.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07098213B2 |
|---|
| 출처 데이터셋 | uspto-grants-2006_08 |
|---|
| ORD ID | ord-70419371049d4118a56e44f216f0f529 |
|---|
| 출처 메모 | uspto-grants-2006_08 |
|---|
